Potassio isocyanate → N-(4,4-Dimethyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-7-yl)urea

HRID 621416ノート

反応式

HRID 621416 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.[N-:16]=[C:17]=[O:18].[K+]>C(O)(=O)C>[CH3:14][C:6]1([CH3:15])[C:5]2[C:10](=[CH:11][C:2]([NH:1][C:17]([NH2:16])=[O:18])=[CH:3][CH:4]=2)[C:9](=[O:12])[NH:8][C:7]1=[O:13]

参加物

4

反応物 2

HCID 11051572Potassio isocyanateHCID 135581517-amino-4,4-dimethylisoquinoline-1,3(2H,4H)-dione

生成物 1

HCID 21242858N-(4,4-Dimethyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-7-yl)urea

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1.3 g. (6.3 mMole) 7-amino-4,4-dimethylisoquinoline-1,3-dione was suspended in 30 ml. 2N acetic acid, mixed with 1.0 g. (12.5 mMole) potassium isocyanate and stirred for 6 hours at 80° C. The reaction mixture was cooled and the precipitate was filtered off with suction and washed with water. The residue was dissolved in dilute aqueous sodium hydroxide solution, the solution was neutralised with dilute hydrochloric acid, the residue was filtered off with suction and, for purification, worked up with ethanol and filtered off with suction. Yield: 0.6 g. (38.5% of theory); m.p. 260°-264° C.

後処理

  1. temperatureThe reaction mixture was cooled
  2. filtrationthe precipitate was filtered off with suction
  3. washwashed with water
  4. dissolutionThe residue was dissolved in dilute aqueous sodium hydroxide solution
  5. filtrationthe residue was filtered off with suction and, for purification
  6. filtrationfiltered off with suction

出典と根拠

ORDレコード
ord-e606f20b4a8b483aa06baaab95ff68a3
出典データセット
uspto-grants-1989_04
特許番号
US04824835

反応ノート

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