HRID493452

反应详情

EQUATION

反应方程式

HRID 493452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (4S,5S)-2-Allyl-2-chloro-3,4-dimethyl-5-phenyl-[1,3,2]oxazasilolidine (2.08 g, 7.8 mmol) in methylene chloride (25 mL) was added triethylamine (1.2 mL, 8.6 mmol). 2-Propanol (0.6 mL, 7.8 mmol) was added slowly by syringe and the mixture was allowed to stir for 12 hours. The methylene chloride was removed by distillation and pentane (20 ml) was added to the residue. The mixture was stirred for 3 hours. The mixture was then filtered through a pad of celite. The filtrate was concentrated to afford an oil which was distilled under reduced pressure (b.p. ˜72° C., ˜0.2 mm Hg) to yield 1.08 g (48%) of (4S,5S)-2-Allyl-2-isopropoxy-3,4-dimethyl-5-phenyl-[1,3,2]oxazasilolidine as a ˜2:1 mixture of diastereomers.

WORKUP

后处理

  1. customThe methylene chloride was removed by distillation and pentane (20 ml)
  2. additionwas added to the residue
  3. stirringThe mixture was stirred for 3 hours
  4. filtrationThe mixture was then filtered through a pad of celite
  5. concentrationThe filtrate was concentrated
  6. customto afford an oil which
  7. distillationwas distilled under reduced pressure (b.p. ˜72° C., ˜0.2 mm Hg)