تفاعل #93967

معادلة التفاعل

Dimethyl sulphate

12b-hydroxy-10,11-dimethoxy-5,6,8,12b-tetrahydroisoindolo[1,2-a]isoquinol-8-one

→

1-(4,5-Dimethoxy-2-methoxycarbonylphenyl)-3,4-dihydroisoquinoline

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture is heated
2. 2
   درجة الحرارةunder reflux for 6 hours
3. 3
   تركيزAfter concentration to 100 cc
4. 4
   workup.ADDITIONthe successive addition of water (300 cc)
5. 5
   استخلاصof 10N sodium hydroxide (70 cc), the mixture is extracted three times with ethyl acetate (total 400 cc)
6. 6
   غسيلThe combined organic solutions are washed three times with distilled water (total 400 cc)
7. 7
   تجفيفdried over anhydrous sodium sulphate
8. 8
   workup.ADDITIONtreated with decolourising charcoal (1 g)
9. 9
   ترشيحfiltered
10. 10
    أخرىevaporated

الإجراء التجريبي

Dimethyl sulphate (48 cc) is added to a suspension of 12b-hydroxy-10,11-dimethoxy-5,6,8,12b-tetrahydroisoindolo[1,2-a]isoquinol-8-one (80.65 g) in methanol (563 cc) and the reaction mixture is heated under reflux for 6 hours. After concentration to 100 cc and the successive addition of water (300 cc) and then of 10N sodium hydroxide (70 cc), the mixture is extracted three times with ethyl acetate (total 400 cc). The combined organic solutions are washed three times with distilled water (total 400 cc), dried over anhydrous sodium sulphate, treated with decolourising charcoal (1 g), filtered and evaporated. 1-(4,5-Dimethoxy-2-methoxycarbonylphenyl)-3,4-dihydroisoquinoline (67.8 g), melting at 133° C., is thus obtained.

المصدر