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

HRID 1451977

反応式

HRID 1451977 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b14709ea61d846a78180e562f3dadce8
出典データセット
uspto-grants-1997_02
特許番号
US05605925

関連ノート

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