反应详情

A 3.7 g. (0.0235 mole) sample of 5-hydroxy-3,4-dihydro-2(1H)-naphthalenone in 125 ml. of methanol is added to a cooled solution of 1.0 g. (0.025 mole) of sodium borohydride in 25 ml. of methanol. After 150 minutes at 0°, 7.2 g. of acetic acid is added and the solvent removed in vacuo. Partitioning between water and methylene chloride gives 3.54 g. of crude product after further extraction, drying and solvent removal. Recrystallization from hexane-ethyl acetate gives 2.92 g., m.p. 126°-128.5°. (lit. m.p. 127°-128°) JACS, 80, 2887 (1958).

1. customthe solvent removed in vacuo
2. customPartitioning between water and methylene chloride
3. customgives 3.54 g
4. extractionof crude product after further extraction
5. customdrying
6. customsolvent removal
7. customRecrystallization from hexane-ethyl acetate
8. customgives 2.92 g