反应详情

The title product of example 12 (1.039 g, 3.18 mmol) was dissolved in 50 mL of tetrahydrofuran, 10 mL of methanol and 5 mL of chloroform at 50° C. Sodium dihydrogen phosphite (NaH2PO2, 3.822 g, 36 mmol) and 10% palladium on carbon (0.19 g) were added followed by dropwise addition of 10 mL of water. When 3 mL of water had been added the mixture became noticeably more homogeneous. After 1 hour the mixture was filtered through Celite. The Celite was washed thoroughly with methanol and chloroform. The combined organic solutions were vacuum evaporated to a residue which was triturated with water, 3% aqueous sodium bicarbonate and filtered. The solid title product was washed with water then diethyl ether and dried in vacuo, 1.054 gm (127%, wet). A portion of the above product was recrystallized from a minimum amount of hot ethanol and water to give, after removal of a small first crop of impure material, pure title product, (43%), mp 180° C. (dec).

1. customat 50° C
2. filtrationAfter 1 hour the mixture was filtered through Celite
3. washThe Celite was washed thoroughly with methanol and chloroform
4. customevaporated to a residue which
5. customwas triturated with water, 3% aqueous sodium bicarbonate
6. filtrationfiltered
7. washThe solid title product was washed with water
8. dry with materialdiethyl ether and dried in vacuo, 1.054 gm (127%, wet)
9. customA portion of the above product was recrystallized from a minimum amount of hot ethanol and water
10. customto give
11. customafter removal of a small first crop of impure material, pure title product, (43%), mp 180° C. (dec)