HRID1603315

反应详情

EQUATION

反应方程式

HRID 1603315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

--Quantities: partially resolved ethyl 2-fluorooctanoate 68 (44 g, 0.23 mol), 0.063M phosphate buffer (pH 7.0) (400 ml), deionised water (400 ml), Pseudomonas lipase (Amano PS) (40 mg). The experimental procedure was as described for compound 66. The hydrolysis was continued until the rate of reaction was almost zero, as indicated by a constant pH with zero addition of alkali (reaction time 5 h, 38 ml of 1M sodium hydroxide solution added i.e. 16% hydrolysis). The mixture was extracted with ether (3 times) and the combined organic solutions were washed with brine, dried (K2CO3) and evaporated. The liquid was distilled to give ethyl (R)-(+)-2-fluoroacetate 69 (30.7 g, 0.23 mol), b.p. 63° C. at 0.6 mm Hg; [α]D26 =+8.5° (c 5.9 in CHCl3).

WORKUP

后处理

  1. customThe hydrolysis was continued until the rate of reaction
  2. extractionThe mixture was extracted with ether (3 times)
  3. washthe combined organic solutions were washed with brine
  4. dry with materialdried (K2CO3)
  5. customevaporated
  6. distillationThe liquid was distilled