反应详情

Potassium cyanide (7.36 g, 113 retool) was added to a solution of 3-dimethylaminomethyl-4-chloro-5-benzyloxy-indole (9.30 g, 29.5 mmol) in sieve-dried DMF (150 ml). Methyl iodide (17.2 g, 121 mmol) was added dropwise, while stirring over 15 minutes, and stirring was continued for a further hour. The mixture was poured into 10% aqueous sodium sulphate and extracted with diethyl ether. The combined extracts were dried (Na2SO4) and evaporated to dryness leaving an oil which crystallised. Recrystallisation from methanol gave 3-cyanomethyl-4-chloro-5-benzyloxyindole (5.56 g), m.p. 130°-2° C.

1. stirringstirring
2. waitwas continued for a further hour
3. extractionextracted with diethyl ether
4. dry with materialThe combined extracts were dried (Na2SO4)
5. customevaporated to dryness
6. customleaving an oil which
7. customcrystallised
8. customRecrystallisation from methanol