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

HRID 745300ノート

反応式

HRID 745300 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-af351d060f564348b9ccb3500af71c87
出典データセット
uspto-grants-1986_07
特許番号
US04598148

反応ノート

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