反应详情

A solution of 4-methylamino-2-methylsulfanyl-5-pyrimidinecarboxylate ethyl ester (4.36 g, 19.3 mmol) in 60 mL of tetrahydrofuran was added dropwise to a room temperature suspension of lithium aluminum hydride (1.10 g, 29.0 mmol) in 40 mL of tetrahydrofuran. After 10 minutes the reaction was carefully quenched with 2 mL of water, 2 mL of 15% NaOH, and an additional 7 mL of water. The mixture was stirred for 1 hour, and the white precipitate which had formed was removed by filtration, and was washed with ethyl acetate. The filtrate was concentrated in vacuo and 3:1 hexane:ethyl acetate was added. The solids were collected to give 2.99 g (84%) of 4-methylamino-2-methylsulfanyl-5-pyrimidinemethanol; mp 155°-157° C.

1. customAfter 10 minutes the reaction was carefully quenched with 2 mL of water, 2 mL of 15% NaOH
2. customthe white precipitate which had formed
3. customwas removed by filtration
4. washwas washed with ethyl acetate
5. concentrationThe filtrate was concentrated in vacuo and 3:1 hexane
6. additionethyl acetate was added
7. customThe solids were collected