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

HRID 453377

反応式

HRID 453377 の反応式
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]

参加物

6

反応物 3

HCID 8857Ethyl AcetateHCID 248232552-methyl-5-nitro-N-(pyrimidin-5-yl)benzamideHCID 178418361HCID 178418361、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A 2L 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.

後処理

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

出典と根拠

ORDレコード
ord-0464d5cdc18f482d940e198df9ce7402
出典データセット
uspto-grants-2013_07
特許番号
US08492404B2

関連ノート

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