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Hydrochloric Acid → (S)-3-amino-5-methanesulfonyl-1-methyl-1,3,4,5-tetrahydro-benzo[b][1,4]diazepin-2-one hydrochloride

HRID 1372968
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HRID 1372968 반응식
C(OC(=O)[NH:7][C@@H:8]1[C:14](=[O:15])[N:13]([CH3:16])[C:12]2[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=2[N:10]([S:21]([CH3:24])(=[O:23])=[O:22])[CH2:9]1)(C)(C)C.[ClH:26]>O1CCOCC1>[ClH:26].[NH2:7][C@@H:8]1[C:14](=[O:15])[N:13]([CH3:16])[C:12]2[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=2[N:10]([S:21]([CH3:24])(=[O:23])=[O:22])[CH2:9]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69043284((S)-5-methanesulfonyl-1-methyl-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 69037713(S)-3-amino-5-methanesulfonyl-1-methyl-1,3,4,5-tetrahydro-benzo[b][1,4]diazepin-2-one hydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
50 °C

실험 절차

A solution of 100 mg (0.27 mmol) of ((S)-5-methanesulfonyl-1-methyl-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-yl)-carbamic acid tert-butyl ester in 5 ml of dioxane was treated with 0.22 ml of hydrochloric acid and heated in the sealed flask at 50° C. for 1 hour. For the working-up, the solvent was evaporated under reduced pressure and the residue submitted to a azeotropic distillation with toluene. After drying under reduced pressure, the (S)-3-amino-5-methanesulfonyl-1-methyl-1,3,4,5-tetrahydro-benzo[b][1,4]diazepin-2-one hydrochloride was obtained in quantitative yield as a light yellow solid; MS: m/e=270 (M+H)+.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. distillationthe residue submitted to a azeotropic distillation with toluene
  3. customAfter drying under reduced pressure

출처 및 근거

ORD 기록
ord-9beba4e721284c14877cc9e048306922
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160875B2

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