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

HRID 2118504

반응식

HRID 2118504 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 222Ammonia용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d8dbedc0f774882852ce542ea9e0af5
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678792

연결된 노트

불러오는 중…