反应详情

To a solution of vacuum dried 10 (225 mg, 0.585 mmol) in methylene chloride (5 mL) bromotrimethyl silane (895 mg, 5.85 mmol) was added and the mixture was stirred at room temperature. TLC showed completion of the reaction after 6 h. Solvents were removed under reduced pressure, and the residue was stirred in 95% methanol (3 mL) for 1 h. The mixture was concentrated under reduced pressure, dried under vacuum to give 150 mg (78%) of 11 as light yellow solid. mp 66–69° C.; 1H NMR (CD3OD): δ 2.03 (m, 2H), 1.59 (m, 2H), 1.24 (br s, 22H), 0.90 (t, J=6.6 Hz, 3H); MS: [M−H]— at m/z 327.3. Anal. (C15H31F2O3P.0.2H2O) C, H.

1. additionwas added
2. customcompletion of the reaction after 6 h
3. customSolvents were removed under reduced pressure
4. stirringthe residue was stirred in 95% methanol (3 mL) for 1 h
5. concentrationThe mixture was concentrated under reduced pressure
6. customdried under vacuum