Water → 1-(1-Amino-1H-pyrrol-2-yl)ethanone

HRID 1080468

반응식

HRID 1080468 반응식
[C:1]([C:4]1[N:5]([N:9]2C(=O)C3C(=CC=CC=3)C2=O)[CH:6]=[CH:7][CH:8]=1)(=[O:3])[CH3:2].CN.O>CN(C)C=O>[NH2:9][N:5]1[CH:6]=[CH:7][CH:8]=[C:4]1[C:1](=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 6329MethylamineHCID 199667522-(2-Acetyl-1H-pyrrol-1-yl)-1H-isoindole-1,3(2H)dione

생성물 1

HCID 199667441-(1-Amino-1H-pyrrol-2-yl)ethanone수율 93.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 2-(2-acetyl-1H-pyrrol-1-yl)-1H-isoindole-1,3(2H)dione (8.53 g) in dimethylformamide (25 ml) was added 33 ml of 40% methylamine solution. After 2.5 hours, the reaction mixture was poured into water (300 ml) and was extracted 4 times with EtOAc. The combined organics were washed once with water and brine, dried (MgSO4), filtered and concentrated to give the crude product. Purification via flash column chromatography (silica gel, 30% EtOAc/hexane) afforded 3.88 g of the product as an oil.

후처리

  1. extractionwas extracted 4 times with EtOAc
  2. washThe combined organics were washed once with water and brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give the crude product
  7. customPurification via flash column chromatography (silica gel, 30% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-49adc91f8f884245bc500069e9b0ce84
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580987

연결된 노트

불러오는 중…