反应详情

The phosphine oxide from (f) above (1.4 g) was dissolved in dihydripyran (20 ml) and benzene (5 ml). p-Toluenesulphonic acid (10 mg) was added. After 20 hr, the mixture was concentrated, added to CH2Cl2 and washed with 5% aqueous NaHCO3 /brine and dried. Evaporation of the solvent gave the crude product (1.8 g) essentially quantitatively as a solid. Recrystallised from acetone. m.p. 146°-148° C.; 1Hnmr δ 8.0-7.3 (m, 10 H, aryl), 4.67 (m, W=6 Hz, THP, C-2'H), 3.67 (m, W=36 Hz, THP, C-6'H2), 1.23 (s, 6H); IR νmax 2950 (m), 1440 (m), 118C (s), cm-1 ; (analysis found: % C, 70.80; H, 7.73; P, 8.54; C22H29O3P requires % C, 70.96; H, 7.85; P, 8.32.

1. concentrationthe mixture was concentrated
2. additionadded to CH2Cl2
3. washwashed with 5% aqueous NaHCO3 /brine
4. customdried
5. customEvaporation of the solvent