反应详情

A solution of Example 6 (6.23 g, 33 mmol) and lithium hydroxide monohydrate (1.45 g, 35 mmol) in tetrahydrofuran (50 mL), water (35 mL), and methanol (14 mL) was stirred for 6.5 hours at room temperature. Water (70 mL) was added, and the reaction mixture was acidified to pH 4 using 2 M HCl and extracted with dichloromethane (5×200 mL). The organics were dried (MgSO4) and the solvent removed in vacuo to give a brown solid. This was dissolved in diethyl ether, heptane was added, and the mixture was stirred overnight. Solvent was removed by syringe to give product as a pale brown solid, 27 mmol, 80%.

1. extractionextracted with dichloromethane (5×200 mL)
2. dry with materialThe organics were dried (MgSO4)
3. customthe solvent removed in vacuo
4. customto give a brown solid
5. customSolvent was removed by syringe
6. customto give product as a pale brown solid, 27 mmol, 80%