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Sodium Sulfate → Ethyl 2-(2,2-difluoroethoxy)-4-methylamino-5-amino-benzoate

HRID 410098
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HRID 410098 반응식
[F:1][CH:2]([F:21])[CH2:3][O:4][C:5]1[CH:15]=[C:14]([NH:16][CH3:17])[C:13]([N+:18]([O-])=O)=[CH:12][C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[O-]S([O-])(=O)=O.[Na+].[Na+]>[Ni].C1COCC1>[NH2:18][C:13]1[C:14]([NH:16][CH3:17])=[CH:15][C:5]([O:4][CH2:3][CH:2]([F:21])[F:1])=[C:6]([CH:12]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24436Sodium SulfateHCID 59529798Ethyl 2-(2,2-difluoroethoxy)-4-(methylamino)-5-nitrobenzoate

생성물 1

HCID 59529827Ethyl 2-(2,2-difluoroethoxy)-4-methylamino-5-amino-benzoate

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of ethyl 2-(2,2-difluoroethoxy)-4-(methylamino)-5-nitrobenzoate (2.0 g; 6.57 mmol), RaNi (1.0 g) and THF (100 mL) is stirred under H2-atmosphere (8 atm) overnight at rt. Na2SO4 is added and the mixture is stirred another 30 min under H2-atmosphere. The mixture is filtered through celite and concentrated and the sub-title compound is used in the next step without further purification.

후처리

  1. stirringthe mixture is stirred another 30 min under H2-atmosphere
  2. filtrationThe mixture is filtered through celite and
  3. concentrationconcentrated
  4. customthe sub-title compound is used in the next step without further purification

출처 및 근거

ORD 기록
ord-08d7e03df07a49da8cbb79d6517aa1cb
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759537B2

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