tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-1-acetate tartrate

Preparation

The preparation of the tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-benaepin-2-one-1-acetate tartrate is as follows:Chiral Resolution Of Highly Pure (+1-T-BUTYLOX CARBONYLMETHYL-3-AMINO- 2, 3, 4N5-TETRAHYDRO-LH-[L] BENZAZEPIN-2-ONE USING Tartaric Acid Part A: Preparation of Highly Pure (S)-L-T-BUTYLOXYCARBONYLMETHYL-3-AMINO- 2,3, 4, 5-Tetrahydro-lh- [l] Benzazepin-2-One Tartrate Salt of Formula V Highly pure 1-t-butyloxycarbonylmethyl-3-amino-2, 3, 4, 5-TETRAHYDRO-LH- BENZAZEPIN-2-ONE of Formula II (5.0 g, 17.24 mmol) was heated in ethanol (12.5 ml) at 50-55°C for 25 minutes. The temperature was further raised to 60-65°C and to this was added a solution of L- (+)-tartaric acid (1.8g, 11.9mmol) in ethanol (7.5ml). The reaction mixture was stirred for 24 hours at 60-65°C, allowed to cool to 35-37°C and filtered at the same temperature to afford the crude product (2.75g, 72%). This was suspended in alcohol (11ml) and stirred at 62-65°C for 3 hours, allowed to cool to 45-47°C and filtered to afford the title compound. Yield: 2.55 g, 93% Purity: 99.87%