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

HRID 745300노트

반응식

HRID 745300 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-af351d060f564348b9ccb3500af71c87
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04598148

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