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Sodium Hydroxide → Amlodipine

HRID 1840423
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HRID 1840423 반응식
[CH3:1][CH2:2][O:3][C:4]([C:6]1[CH:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=2[Cl:18])[C:10]([C:19]([O:21][CH3:22])=[O:20])=[C:9]([CH3:23])[NH:8][C:7]=1[CH2:24][O:25][CH2:26][CH2:27][NH2:28])=[O:5].C1C=CC(S(O)(=O)=O)=CC=1.[OH-].[Na+]>ClCCl.O>[CH3:1][CH2:2][O:3][C:4]([C:6]1[CH:11]([C:12]2[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:10]([C:19]([O:21][CH3:22])=[O:20])=[C:9]([CH3:23])[NH:8][C:7]=1[CH2:24][O:25][CH2:26][CH2:27][NH2:28])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 60496Amlodipine Besylate

생성물 1

HCID 2162Amlodipine수율 93.8%

시약·촉매·용매 1

HCID 21908982Water methylene chloride용매

실험 절차

Amlodipine besylate (30 g) was slurried into a mixture of dichloromethane/water (1:1, 500 ml) and the rapidly slurred emulsion was basified to pH 11 with aqueous sodium hydroxide (5M). The resulting organic layer was separated and the remaining aqueous layer extracted with dichloromethane (100 ml). The combined extracts were washed with water (150 ml) dried (MgSO4) and evaporated in vacuo to afford an off-white solid (20.3 g).

후처리

  1. customThe resulting organic layer was separated
  2. extractionthe remaining aqueous layer extracted with dichloromethane (100 ml)
  3. washThe combined extracts were washed with water (150 ml)
  4. dry with materialdried (MgSO4)
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-51803a9efd024ddfb0e9ab5fa71acbc8
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680334B2

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