Sodium Hydroxide → Ethyl 3-allyloxycarbonylamino-3-(3-[3-aminophenylsulphonylamino]-phenyl)-propionate

HRID 968470노트

반응식

HRID 968470 반응식
[Sn](Cl)Cl.[CH2:4]([O:7][C:8]([NH:10][CH:11]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([NH:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([N+:34]([O-])=O)[CH:29]=2)(=[O:27])=[O:26])[CH:19]=1)[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH:5]=[CH2:6].[OH-].[Na+]>C(O)C>[CH2:4]([O:7][C:8]([NH:10][CH:11]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([NH:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([NH2:34])[CH:29]=2)(=[O:27])=[O:26])[CH:19]=1)[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH:5]=[CH2:6]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 21101499Ethyl 3-allyloxycarbonylamino-3-(3-[3-nitrophenylsulphonylamino]-phenyl)-propionate

생성물 1

HCID 21101498Ethyl 3-allyloxycarbonylamino-3-(3-[3-aminophenylsulphonylamino]-phenyl)-propionate수율 55.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

43.5 g of tin-(II) chloride were added to a solution of 17.8 g of ethyl 3-{[(allyloxy)-carbonyl]-amino}-3-{{3-{[(3-nitrophenyl)-sulfonyl]-amino}-phenyl}}-propanoate from Example II.2.e in 165 ml of ethanol, and the mixture was heated to reflux for a period of time of 2 h. The reaction mixture was hydrolized with 200 ml of aqueous 2N sodium hydroxide solution, then filtered through silica gel and washed with dichloromethane. The organic phase was dried over magnesium sulphate and concentrated to yield 9.2 g of a solid.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for a period of time of 2 h
  3. filtrationfiltered through silica gel
  4. washwashed with dichloromethane
  5. dry with materialThe organic phase was dried over magnesium sulphate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-67c4c1bf1eba46ac9556a04389c7aae6
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304037B2

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