Chlorosuccinimide → HCID 19892016、化合物

HRID 893261ノート

反応式

HRID 893261 の反応式
[C:1]1([CH:7]2[CH2:16][CH2:15][C:14]3[C:9]4=[C:10]([C:17](=[O:20])[C:18](=[O:19])[N:8]24)[CH:11]=[CH:12][CH:13]=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:21]N1C(=O)CCC1=O>CN(C)C=O>[Cl:21][C:12]1[CH:13]=[C:14]2[C:9]3=[C:10]([C:17](=[O:20])[C:18](=[O:19])[N:8]3[CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:16][CH2:15]2)[CH:11]=1

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 14988427HCID 14988427、化合物

生成物 1

HCID 19892016HCID 19892016、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of 5,6-dihydro-4-phenyl-4H-pyrrolo[3,2,1-ij]-quinoline-1,2-dione (3.1 g) and N-chlorosuccinimide (1.89 g) in dimethylformamide (DMF; 50 ml) was stirred at 80 ° C. for an hour. After cooling, the mixture was concentrated under reduced pressure and to the resulting residue was added chloroform (500 ml). The organic layer was washed with water and saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated under reduced pressure to give the title compound (3.4 g, 96.8%). This crystals was recrystallized from acetonitrile to give dark reddish crystals, mp 173°-174 ° C.

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated under reduced pressure and to the resulting residue
  3. additionwas added chloroform (500 ml)
  4. washThe organic layer was washed with water and saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-98f45929e1514f92aac225c621720518
出典データセット
uspto-grants-1992_06
特許番号
US05124325

反応ノート

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