Ammonium formate → HCID 43376334, 화합물

HRID 2381690노트

반응식

HRID 2381690 반응식
[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

참가 물질

6

반응물 2

HCID 2723923Ammonium formateHCID 66877507HCID 66877507, 화합물

생성물 1

HCID 43376334HCID 43376334, 화합물수율 53%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5c87067505f145259b40bdef68e9303c
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258144B2

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