Ethyl Acetate → 5-amino-2-methyl-N-(pyrimidin-5-yl)benzamide

HRID 2355096

반응식

HRID 2355096 반응식
CCOC(C)=O.[CH3:7][C:8]1[CH:22]=[CH:21][C:20]([N+:23]([O-])=O)=[CH:19][C:9]=1[C:10]([NH:12][C:13]1[CH:14]=[N:15][CH:16]=[N:17][CH:18]=1)=[O:11].[H][H]>CO.[Pd]>[NH2:23][C:20]1[CH:21]=[CH:22][C:8]([CH3:7])=[C:9]([CH:19]=1)[C:10]([NH:12][C:13]1[CH:18]=[N:17][CH:16]=[N:15][CH:14]=1)=[O:11]

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 248232552-methyl-5-nitro-N-(pyrimidin-5-yl)benzamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 248240475-amino-2-methyl-N-(pyrimidin-5-yl)benzamide

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A 2 L high-pressure vessel was charged with Palladium 10% on carbon wet (50% water) and EtOAc (50 mL). 2-methyl-5-nitro-N-(pyrimidin-5-yl)benzamide 45 (18.79 g) was dissolved in methanol (400 mL) and added to the previous mixture. The reaction vessel was pressurized to 30 psi of H2 and mechanically stirred until the hydrogen intake stopped. The reduction of the nitro group was complete by LCMS and the mixture was filtered off through paper and glass paper. The crude 5-amino-2-methyl-N-(pyrimidin-5-yl)benzamide 46 was obtained as a yellow solid and used without further purification.

후처리

  1. additionadded to the previous mixture
  2. filtrationthe mixture was filtered off through paper and glass paper

출처 및 근거

ORD 기록
ord-cf248572e410495aab32c2cbe1551cb3
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754717B2

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