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Water → Amlodipine

HRID 2180022
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HRID 2180022 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.O.[OH-].[Na+]>C(Cl)Cl>[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

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 60496Amlodipine Besylate

생성물 1

HCID 2162Amlodipine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a slight suspension of racemic amlodipine besylate (100.37 g, 0.177 mol) [prepared by the method described in European Patent No. 0244944] in methylene chloride (250 mL, 2.5 mL/g) and water (250 mL, 2.5 mL/g) was added 11 M sodium hydroxide (24 mL) to achieve pH 13-14. The mixture was stirred for ten minutes during which time it became a solution. The layers were separated and the organic layer washed with water (1×250 mL) and gravity filtered through a magnesium sulphate (25 g) bed. The magnesium sulphate was washed with methylene chloride (40 mL) and to the combined filtrates was added dimethyl sulphoxide (360 mL). The methylene chloride was removed on a rotary evaporator (45 minutes on a water aspirator followed by 15 minutes under high vacuum).

후처리

  1. customprepared by the method
  2. customThe layers were separated
  3. washthe organic layer washed with water (1×250 mL) and gravity
  4. filtrationfiltered through a magnesium sulphate (25 g) bed
  5. washThe magnesium sulphate was washed with methylene chloride (40 mL) and to the combined filtrates
  6. additionwas added dimethyl sulphoxide (360 mL)
  7. customThe methylene chloride was removed on a rotary evaporator (45 minutes on a water

출처 및 근거

ORD 기록
ord-386b996615f54ca8883ab09216eaf25e
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06887886B2

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