N-[2-(3,4-dimethoxyphenyl)ethyl]formamide → 3,4-Dihydro-6,7-dimethoxyisoquinoline

HRID 2118504

反応式

HRID 2118504 の反応式
[CH:1]([NH:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][CH3:15])[CH:7]=1)=O>N>[CH3:15][O:14][C:8]1[CH:7]=[C:6]2[C:11](=[CH:10][C:9]=1[O:12][CH3:13])[CH:1]=[N:3][CH2:4][CH2:5]2

参加物

3

反応物 1

HCID 84337N-[2-(3,4-dimethoxyphenyl)ethyl]formamide

生成物 1

HCID 300583,4-Dihydro-6,7-dimethoxyisoquinoline

試薬・触媒・溶媒 1

HCID 222Ammonia溶媒

反応条件

温度
140 °C

実験手順

The N-formyl-2(3,4-dimethoxy-phenyl)-ethylamine so obtained is stirred with polyphosphoric acid (1 kg) and heated to 140° C. (oil bath temperature). The reaction mixture foams vigorously starting from an internal temperature of 70° C. After 30 minutes, an internal temperature of about 140° C. is attained. The mixture is then poured onto water (1 liter) and made alkaline with concentrated ammonia (1.8 liters) while ice is added. The reaction product is extracted repeatedly with ethyl acetate, the ethyl acetate phase is washed with water, dried, over magnesium sulphate and evaporated giving the title compound (142.5 g) as an oil.

後処理

  1. customvigorously starting from an internal temperature of 70° C
  2. customan internal temperature of about 140° C.
  3. additionThe mixture is then poured onto water (1 liter)
  4. additionis added
  5. extractionThe reaction product is extracted repeatedly with ethyl acetate
  6. washthe ethyl acetate phase is washed with water
  7. dry with materialdried, over magnesium sulphate
  8. customevaporated

出典と根拠

ORDレコード
ord-6d8dbedc0f774882852ce542ea9e0af5
出典データセット
uspto-grants-1987_07
特許番号
US04678792

関連ノート

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