Dimethylcarbamoyl Chloride → N,N-Dimethyl-N'-(4,4-dimethyl-1,2,3,4-tetrahydro-1,3-dioxo-7-isoquinolinyl)-urea

HRID 621419

반응식

HRID 621419 반응식
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:15])([CH3:14])[C:7](=[O:13])[NH:8][C:9]2=[O:12])=[CH:4][CH:3]=1.[CH3:16][N:17]([CH3:21])[C:18](Cl)=[O:19]>N1C=CC=CC=1>[CH3:16][N:17]([CH3:21])[C:18]([NH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:15])([CH3:14])[C:7](=[O:13])[NH:8][C:9]2=[O:12])=[CH:4][CH:3]=1)=[O:19]

참가 물질

4

반응물 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 135581517-amino-4,4-dimethylisoquinoline-1,3(2H,4H)-dione

생성물 1

HCID 21242848N,N-Dimethyl-N'-(4,4-dimethyl-1,2,3,4-tetrahydro-1,3-dioxo-7-isoquinolinyl)-urea

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1.3 g. (6.3 mMole) 7-amino-4,4-dimethylisoquinoline-1,3-dione was dissolved in 30 ml. pyridine, mixed, while cooling with ice, with 1.5 g. dimethylcarbamoyl chloride and the reaction mixture further stirred for 4 hours at 25° C. Subsequently, the reaction mixture was distilled to dryness, the residue was taken up in methylene chloride, washed with water, dried and the methylene chloride distilled off. The residue was recrystallised from ethanol. Yield 1.1 g. (63.6% of theory); m.p. 256°-258° C.

후처리

  1. temperaturewhile cooling with ice, with 1.5 g
  2. distillationSubsequently, the reaction mixture was distilled to dryness
  3. washwashed with water
  4. customdried
  5. distillationthe methylene chloride distilled off
  6. customThe residue was recrystallised from ethanol

출처 및 근거

ORD 기록
ord-d46dd2ee7094491f8ac07da2da6b03eb
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824835

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