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

HRID 621416노트

반응식

HRID 621416 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.[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e606f20b4a8b483aa06baaab95ff68a3
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824835

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