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Hydrochloric Acid → HCID 18001027, 화합물

HRID 1870446
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HRID 1870446 반응식
C([O:3][C:4]([CH2:6][CH:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[N:11]([C:19](=[O:32])[C:20]2[CH:25]=[CH:24][C:23]([CH:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[CH:22][CH:21]=2)[CH2:10][CH2:9][CH2:8]1)=[O:5])C.[OH-].[Na+].Cl>C(O)C>[C:4]([CH2:6][CH:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[N:11]([C:19](=[O:32])[C:20]2[CH:25]=[CH:24][C:23]([CH:26]3[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]3)=[CH:22][CH:21]=2)[CH2:10][CH2:9][CH2:8]1)([OH:5])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18001046HCID 18001046, 화합물

생성물 1

HCID 18001027HCID 18001027, 화합물수율 95.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-ethoxycarbonylmethyl-7-chloro-1-(4-cyclohexyl-benzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (2 g) in ethanol (20 ml) is added a 5N aqueous sodium hydroxide solution (5 ml), and the mixture is stirred at room temperature overnight. The reaction solution is acidified with hydrochloric acid, and the mixture is extracted with dichloromethane. The extract is washed with water, dried over magnesium sulfate, and evaporated to remove the solvent to give 5-carboxymethyl-7-chloro-1-(4-cyclohexylbenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (1.8 g) in colorless amorphous.

후처리

  1. extractionthe mixture is extracted with dichloromethane
  2. washThe extract is washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customto remove the solvent

출처 및 근거

ORD 기록
ord-03e51653ecd946199b4c03709b141f50
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06096735

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