Sodium Hydroxide → 2-(6,7-Dimethoxy-3,4-dihydroisoquinolin-1(2H)-ylidene)acetamide

HRID 1979716노트

반응식

HRID 1979716 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9](=[CH:15][C:16]#[N:17])[NH:8][CH2:7][CH2:6]2.[OH-:18].[Na+]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9](=[CH:15][C:16](=[O:18])[NH2:17])[NH:8][CH2:7][CH2:6]2

참가 물질

3

반응물 2

HCID 14798Sodium HydroxideHCID 4193891-Cyanomethylene-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline

생성물 1

HCID 704697252-(6,7-Dimethoxy-3,4-dihydroisoquinolin-1(2H)-ylidene)acetamide

실험 절차

Polyphosphoric acid (10.0 g) is heated to 100° C. and 1.0 g of 6,7-dimethoxy-1-cyanomethylene-1,2,3,4-tetrahydroisoquinoline is added under mechanical stirring. The reaction mixture is heated for 1 hour, poured into crushed ice and made basic with 30% sodium hydroxide. The mixture is extracted with chloroform and the extract dried over anhydrous sodium sulfate. The solvent is evaporated under reduced pressure to give a white solid, yield 0.7 g, mp. 156°-158° C.

후처리

  1. temperatureThe reaction mixture is heated for 1 hour
  2. additionpoured
  3. custominto crushed ice
  4. extractionThe mixture is extracted with chloroform
  5. dry with materialthe extract dried over anhydrous sodium sulfate
  6. customThe solvent is evaporated under reduced pressure
  7. customto give a white solid, yield 0.7 g, mp. 156°-158° C.

출처 및 근거

ORD 기록
ord-cf7b7e0ab3834c05ae019129caa89e01
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482556

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