HRID1948148

反应详情

EQUATION

反应方程式

HRID 1948148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 2-methyl-propane-2-sulfinic acid 1-(8-cyclopropylmethyl-1,4-dioxa-spiro[4.5]dec-8-yl)-methylideneamide (19, 1.00 g, 3.05 mmol) in tetrahydrofuran was cooled to −40° C. and was treated sequentially with tetramethylammonium fluoride (313 mg, 3.36 mmol, 1.1 eq.) and (trifluoromethyl)trimethylsilane (587 μL, 3.97 mmol, 1.3 eq.). The mixture was stirred for 2 h at 0° C. before being quenched by addition of saturated aqueous ammonium chloride solution and extracted twice with ethyl acetate. The combined organic layers were dried over magnesium sulphate, filtered, and concentrated in vacuo to give 960 mg of the title compound. Rt=1.63 min (Method B). Detected mass: 398.3 (M+H+).

WORKUP

后处理

  1. custombefore being quenched by addition of saturated aqueous ammonium chloride solution
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe combined organic layers were dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo