反应详情

To a stirred and ice-cooled solution of Compound 8 (650 mg, 2.5 mmol) in dry CH2Cl2 (15 ml) was added neat TiCl4 (950 mg, 5.0 mmol) followed by Cl2CHOMe (600 mg, 5.0 mmol). After the addition was complete, the mixture was stirred at room temperature for 5 hr, poured into H2O (60 ml), and extracted with CH2Cl2. The combined extracts were dried (Na2SO4), and concentrated in vacuo to give a yellow oil, which was purified by a column chromatography on silica gel to give Compound 9 (650 mg, 90%)

1. additionAfter the addition
2. stirringthe mixture was stirred at room temperature for 5 hr
3. extractionextracted with CH2Cl2
4. dry with materialThe combined extracts were dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customto give a yellow oil, which
7. customwas purified by a column chromatography on silica gel