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Sodium Hydroxide → HCID 70124887, 화합물

HRID 1596343
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HRID 1596343 반응식
[CH:1]12[CH2:9][CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][N:3]([C:10]([CH2:12][N:13]1[C:19]3[C:20]([CH3:24])=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]([CH2:25][O:26]C(=O)C)=[N:16][CH:15]([NH:30][C:31]([O:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[C:14]1=[O:41])=[O:11])[CH2:2]2.[OH-].[Na+]>C(O)C>[CH:5]12[CH2:8][CH2:9][CH:1]([CH2:7][CH2:6]1)[CH2:2][N:3]([C:10]([CH2:12][N:13]1[C:19]3[C:20]([CH3:24])=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]([CH2:25][OH:26])=[N:16][CH:15]([NH:30][C:31]([O:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[C:14]1=[O:41])=[O:11])[CH2:4]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 54535690HCID 54535690, 화합물

생성물 1

HCID 70124887HCID 70124887, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (3RS)-1-[(3-azabicyclo[3.2.2]non-3-yl)carbonylmethyl]-3-benzyloxycarbonylamino-5-acetoxymethyl-9-methyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one (1.9 g) in ethanol (40 ml) was added 1N-sodium hydroxide solution (7 ml) under stirring at ambient temperature. The mixture was stirred for 20 minutes under the same conditions. After removal of the solvent water was added into the mixture, which was adjusted to pH 4 with a diluted hydrochloric acid and extracted with ethyl acetate twice. The combined extract was washed with water and dried over magnesium sulfate. Removal of the solvent gave (3RS)-1-[(3-azabicyclo[3.2.2]non-3-yl)carbonylmethyl]-3-benzyloxycarbonylamino-5-hydroxymethyl-9-methyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one as an amorphous mass (1.68 g, 95.3%).

후처리

  1. stirringThe mixture was stirred for 20 minutes under the same conditions
  2. customAfter removal of the solvent water
  3. additionwas added into the mixture, which
  4. extractionextracted with ethyl acetate twice
  5. extractionThe combined extract
  6. washwas washed with water
  7. dry with materialdried over magnesium sulfate
  8. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-f93f801e48f84000a1786a120b3acd6c
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06291452B1

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