Chlorosuccinimide → HCID 19892016, 화합물

HRID 893261노트

반응식

HRID 893261 반응식
[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

참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 14988427HCID 14988427, 화합물

생성물 1

HCID 19892016HCID 19892016, 화합물수율 97%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98f45929e1514f92aac225c621720518
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124325

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