Ammonium formate → HCID 43376334、化合物

HRID 2381690ノート

反応式

HRID 2381690 の反応式
[CH2:1]([O:8][CH2:9][C:10]([N:12]([CH3:22])[C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[CH:15][CH:14]=1)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])=O.[NH4+]>CCO.O.[Fe]>[CH2:1]([O:8][CH2:9][C:10]([N:12]([CH3:22])[C:13]1[CH:14]=[CH:15][C:16]([NH2:19])=[CH:17][CH:18]=1)=[O:11])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 2

HCID 2723923Ammonium formateHCID 66877507HCID 66877507、化合物

生成物 1

HCID 43376334HCID 43376334、化合物収率 53%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a suspension of above 2-benzoxy-N-methyl-N-(4-nitrophenyl)acetamide in EtOH (8 mL) and H2O (4 mL) was added ammonium formate (1.3 g, 20 mmol) and Fe (0.47 g, 8.4 mmol). After heating at reflux for 2 h, the reaction was cooled to room temperature, iron was filtered off, and the filtrate was diluted with EtOAc and water, EtOAc layer was separated and the aqueous layer was further extracted with EtOAc, organic layers were combined, dried over Na2SO4, and was concentrated under vacuo to provide 2-benzoxy-N-methyl-N-(4-aminophenyl)acetamide (0.4 g, 53%).

後処理

  1. temperatureAfter heating
  2. temperatureat reflux for 2 h
  3. filtrationiron was filtered off
  4. additionthe filtrate was diluted with EtOAc and water, EtOAc layer
  5. customwas separated
  6. extractionthe aqueous layer was further extracted with EtOAc, organic layers
  7. dry with materialdried over Na2SO4
  8. concentrationwas concentrated under vacuo

出典と根拠

ORDレコード
ord-5c87067505f145259b40bdef68e9303c
出典データセット
uspto-grants-2012_09
特許番号
US08258144B2

反応ノート

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