反応 #2205686

反応方程式

N-formyl-2(3,4-dimethoxy-phenyl)-ethylamine

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title compound

6,7-Dimethoxy-3,4-dihydroisoquinoline

溶媒

ammonia

反応条件

後処理

1. 1
   その他vigorously starting from an internal temperature of 70° C
2. 2
   その他an internal temperature of about 140° C.
3. 3
   workup.ADDITIONThe mixture is then poured onto water (1 liter)
4. 4
   workup.ADDITIONis added
5. 5
   抽出The reaction product is extracted repeatedly with ethyl acetate
6. 6
   洗浄the ethyl acetate phase is washed with water
7. 7
   乾燥dried, over magnesium sulphate
8. 8
   その他evaporated

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.

出典