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

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

Product Name:
tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-1-acetate tartrate
Synonyms:
  • tert-butyl 2-(3-amino-2-oxo-4,5-dihydro-3H-1-benzazepin-1-yl)acetate,2,3-dihydroxybutanedioic acid
  • 1H-1-Benzazepine-1-acetic acid, 3-aMino-2,3,4,5-tetrahydro-2-oxo-, 1,1-diMethylethyl ester, (3S)-, (2R,3R)-2,3-dihydroxybutanedioate (1:1) (9CI)
  • (S)-tert-Butyl 2-(3-aMino-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-1-yl)acetate (2R,3R)-2,3-dihydroxysuccinate
  • tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-1-acetate tartrate
  • T-BUTYL 3S-AMINO-2,3,4,5-TETRAHYDRO-1H-1BENAEPIN-2-ONE-1-ACETATE-TARTRATE
  • tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-...
CAS:
117770-66-8
MF:
C16H22N2O3.C4H6O6
MW:
440.446
EINECS:
1533716-785-6
Mol File:
117770-66-8.mol
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tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-1-acetate tartrate Chemical Properties

Melting point:
190°C (dec.)
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tert-Butyl 3S-amino-2,3,4,5-tetrahydro-1H-[1]benaepin-2-one-1-acetate tartrate Usage And Synthesis

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%

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