Betamethasone 17-valerate(2152-44-5) IR Spectrum

Mass

MS-IW-3431          
9-fluoro-11beta,17,21-trihydroxy-16beta-methyl-1,4-pregnadiene-3,20-dione 17-monovalerate
C27H37FO6           (Mass of molecular ion:    476)

   Source Temperature: 190 °C
   Sample Temperature: 220 °C
   Direct, 75 eV

      17.0       1.0
      18.0       4.1
      26.0       1.2
      27.0      10.3
      28.0       5.1
      29.0      20.0
      30.0       1.2
      31.0       4.6
      39.0       8.9
      40.0       1.6
      41.0      33.1
      42.0       6.2
      43.0      17.7
      44.0       1.0
      45.0       5.4
      51.0       2.6
      52.0       1.3
      53.0       7.9
      54.0       1.2
      55.0      19.9
      56.0       4.7
      57.0      47.9
      58.0       2.6
      59.0       2.7
      60.0      60.6
      61.0       3.0
      63.0       1.0
      65.0       5.5
      66.0       1.3
      67.0       8.2
      68.0       1.2
      69.0       9.5
      70.0       1.1
      71.0       2.7
      73.0      26.2
      74.0       2.8
      75.0       1.6
      77.0      15.5
      78.0       3.3
      79.0      11.5
      80.0       1.8
      81.0       6.6
      82.0       1.4
      83.0       5.2
      84.0       1.4
      85.0      53.8
      86.0       3.3
      87.0       2.9
      88.0       1.5
      89.0       1.4
      91.0      28.0
      92.0       5.9
      93.0      12.7
      94.0       3.6
      95.0      11.7
      96.0       2.4
      97.0       4.0
      99.0       2.0
     101.0       2.4
     102.0       1.3
     103.0       4.7
     104.0       1.6
     105.0      10.6
     106.0       2.8
     107.0      22.6
     108.0       8.5
     109.0      13.7
     110.0       2.6
     111.0       5.0
     112.0       1.4
     113.0       3.2
     114.0       1.4
     115.0       8.5
     116.0       3.6
     117.0       6.7
     118.0       1.7
     119.0       8.2
     120.0       6.0
     121.0     100.0
     122.0      63.9
     123.0      13.0
     124.0       2.8
     125.0       6.1
     126.0       1.2
     127.0       4.4
     128.0       5.0
     129.0       5.1
     130.0       2.3
     131.0       8.0
     132.0       2.8
     133.0      12.8
     134.0      10.1
     135.0      39.0
     136.0       7.7
     137.0       8.1
     138.0       2.3
     139.0       5.7
     140.0       1.6
     141.0       4.8
     142.0       2.3
     143.0       4.0
     144.0       3.1
     145.0      10.5
     146.0       7.9
     147.0      35.8
     148.0       6.1
     149.0       5.6
     150.0       2.7
     151.0       4.7
     152.0       7.5
     153.0       7.2
     154.0       1.9
     155.0       3.2
     156.0       1.3
     157.0       6.6
     158.0       4.4
     159.0      17.6
     160.0      16.9
     161.0      15.5
     162.0       3.7
     163.0       6.6
     164.0       2.4
     165.0       6.6
     166.0       2.7
     167.0       3.2
     168.0       1.3
     169.0       3.2
     170.0       1.7
     171.0      13.6
     172.0       5.1
     173.0      10.6
     174.0       3.7
     175.0      10.9
     176.0       3.2
     177.0       5.6
     178.0       3.3
     179.0       5.8
     180.0       1.8
     181.0       3.4
     182.0       1.5
     183.0       3.1
     184.0       2.7
     185.0       7.8
     186.0       5.4
     187.0      15.1
     188.0       3.6
     189.0      11.7
     190.0       3.0
     191.0       5.7
     192.0       1.8
     193.0       3.9
     194.0       2.1
     195.0       7.5
     196.0       2.6
     197.0       4.7
     198.0       2.0
     199.0       3.9
     200.0       1.7
     201.0       2.4
     202.0       3.2
     203.0       4.6
     204.0       1.9
     205.0       4.2
     206.0       1.6
     207.0       4.2
     208.0       4.3
     209.0       5.5
     210.0       2.6
     211.0       5.2
     212.0       2.3
     213.0       6.1
     214.0       2.2
     215.0       3.0
     216.0       1.0
     217.0       1.9
     219.0       1.7
     220.0       1.1
     221.0       3.5
     222.0       2.5
     223.0      13.9
     224.0       6.3
     225.0       7.3
     226.0       4.4
     227.0       3.9
     228.0       1.4
     229.0       1.6
     231.0       1.3
     233.0       2.3
     234.0       1.3
     235.0       3.2
     236.0       3.6
     237.0       6.7
     238.0       4.6
     239.0       6.4
     240.0       3.2
     241.0       5.0
     242.0       3.3
     243.0       2.7
     244.0       1.4
     245.0       1.4
     247.0       2.1
     248.0       1.7
     249.0       2.6
     250.0       1.5
     251.0       3.5
     252.0       1.9
     253.0       6.6
     254.0       3.2
     255.0       4.2
     256.0       1.8
     257.0       2.0
     258.0       1.0
     259.0       1.5
     260.0       1.3
     261.0       2.7
     262.0       3.8
     263.0       4.3
     264.0       2.2
     265.0       3.4
     266.0       2.2
     267.0       7.7
     268.0       2.9
     269.0       2.6
     273.0       1.0
     274.0       1.2
     275.0       2.8
     276.0       1.9
     277.0      18.4
     278.0       6.9
     279.0      26.7
     280.0       7.1
     281.0       4.0
     282.0       8.2
     283.0       3.0
     284.0       1.9
     285.0       1.9
     289.0       1.4
     290.0       1.7
     291.0       1.7
     292.0       1.2
     293.0       3.3
     294.0       2.3
     295.0      31.6
     296.0       8.8
     297.0      14.3
     298.0       4.4
     299.0       2.5
     301.0       1.0
     303.0       1.4
     304.0       1.9
     305.0       1.9
     306.0       1.3
     307.0       5.1
     308.0       3.9
     309.0       2.2
     310.0       1.8
     311.0       2.3
     312.0       4.3
     313.0       8.4
     314.0       3.1
     315.0      93.6
     316.0      21.4
     317.0       3.8
     318.0       1.5
     319.0       1.0
     321.0       2.2
     323.0       7.2
     324.0       3.6
     325.0       8.9
     326.0       4.9
     327.0       2.4
     328.0       1.6
     329.0       2.8
     331.0       1.3
     333.0      17.3
     334.0       4.1
     335.0       1.1
     336.0       2.9
     337.0       1.5
     338.0       1.3
     339.0       2.1
     340.0       1.5
     341.0       2.8
     342.0       7.4
     343.0      70.7
     344.0      17.2
     345.0       9.0
     346.0       2.8
     347.0       1.1
     354.0      11.8
     355.0       3.3
     356.0       1.9
     359.0       1.5
     361.0       4.5
     362.0       3.5
     372.0       1.2
     374.0       4.7
     375.0       1.3
     426.0       2.6
     445.0       7.2
     446.0       2.2
     456.0       2.7
     476.0       1.1

400 MHz in CDCl3

¹H NMR	399.65 MHz
C₂₇ H₃₇ F O₆	0.033 g : 0.5 ml CDCl₃
9-fluoro-11beta,17,21-trihydroxy-16beta-methyl-1,4-pregnadiene-3,20-dione 17-monovalerate

    Assign.     Shift(ppm)

      A             7.255
      B             6.345
      C             6.137
      D             4.426
      E     *1      4.067
      F     *1      4.034
      G             3.25
      J             2.82
      K             2.648
      L             2.50
      M          2.44 to 2.42
      N             2.325
      P             2.153
      Q             2.01
      R             1.95
      S             1.58
      T             1.565
      U             1.405
      V             1.338
      W             1.24
      X             0.963
      Y             0.904
     
     ASSIGNED BY H-H AND C-H COSY

     Hz     ppm     Int.

   2904.79   7.269    168
   2894.65   7.243    175
   2541.99   6.361    133
   2540.16   6.356    135
   2531.86   6.336    129
   2530.03   6.331    135
   2452.64   6.137    176
   2451.17   6.134    107
   1774.90   4.442     39
   1772.22   4.435     41
   1769.29   4.428     37
   1766.24   4.420     41
   1763.67   4.414     41
   1638.18   4.100     33
   1624.76   4.066    131
   1620.24   4.055    142
   1618.16   4.049    131
   1612.55   4.035    128
   1594.60   3.990     30
   1303.59   3.262     85
   1299.07   3.251    110
   1298.10   3.249    136
   1293.70   3.238     82
   1128.66   2.825     73
   1125.85   2.818    125
   1123.05   2.811     77
   1063.23   2.661     35
   1061.89   2.658     36
   1057.25   2.646     37
   1055.79   2.642     36
    987.92   2.472     34
    987.43   2.471     34
    984.13   2.463     62
    969.85   2.427     99
    967.53   2.421     84
    959.72   2.402     47
    959.23   2.401     47
    955.20   2.391     46
    937.50   2.346    156
    930.18   2.328    226
    922.36   2.308    202
    865.60   2.166     44
    857.91   2.147     44
    856.57   2.144     41
    804.32   2.013     30
    798.46   1.998     48
    789.06   1.975     63
    786.38   1.968     51
    783.69   1.961     63
    781.13   1.955    124
    772.71   1.934     67
    766.36   1.918     59
    648.68   1.624     57
    647.34   1.620     56
    641.60   1.606     96
    640.01   1.602     85
    638.67   1.599     62
    633.79   1.586    146
    625.49   1.566   1000
    617.43   1.545    105
    601.93   1.507     61
    565.06   1.414    328
    557.74   1.396    318
    552.73   1.384     50
    545.29   1.365    102
    537.84   1.346    145
    530.15   1.327    144
    522.83   1.309     91
    515.50   1.290     32
    499.63   1.251     42
    498.54   1.248     41
    488.65   1.223     41
    384.89   0.964    609
    368.90   0.924    375
    361.57   0.905    784
    354.25   0.887    318

in CDCl3

KBr disc

nujol mull