反应详情

温度

0 °C

2-Methoxypyridine (1.9 ml) and then diisopropylamine (0.1 ml) were added to a solution of methyl lithium (10 ml of a 1.6M solution in ether) in tetrahydrofuran (20 ml) at −78° C. and the solution was stirred at 0° C. for 18hand then re-cooled to −78° C. A solution of 1,1-dimethylethyl [3-(methoxymethylamino)-3-oxopropyl]-carbamate (1.6 g) in tetrahydrofuran (5 ml) was added slowly and the resultant solution was allowed to warm to −30° C. over 3.5 h, quenched with aqueous ammonium chloride and extracted with ether (three times). The combined organic extracts were dried (sodium sulphate), evaporated and purified by chromatography on silica eluting with petrol-ether gave the sub-title compound as a colourless oil (0.572 g).

1. temperaturethen re-cooled to −78° C
2. temperatureto warm to −30° C. over 3.5 h
3. customquenched with aqueous ammonium chloride
4. extractionextracted with ether (three times)
5. dry with materialThe combined organic extracts were dried (sodium sulphate)
6. customevaporated
7. custompurified by chromatography on silica eluting with petrol-ether