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

HRID 621419

反応式

HRID 621419 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d46dd2ee7094491f8ac07da2da6b03eb
出典データセット
uspto-grants-1989_04
特許番号
US04824835

関連ノート

読み込み中…