HRID2196822

反应详情

EQUATION

反应方程式

HRID 2196822 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 (R)-tert-butyl 1-hydroxypropan-2-ylcarbamate (756 mg, 4.31 mmol) and 4-methylbenzene-1-sulfonyl chloride (905 mg, 4.75 mmol) in ethyl ether (30 mL) was added powdered potassium hydroxide (968 mg, 17.26 mmol) and reaction was refluxed for 2 hr. The reaction mixture was poured into a separatory funnel that contained crushed ice and extracted with ether (2×20 mL). The organics were combined, dried with sodium sulfate, filtered, and concentrated. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.16 (d, J=5.43 Hz, 3 H) 1.38 (s, 9 H) 1.83 (d, J=3.73 Hz, 1 H) 2.17 (d, J=5.76 Hz, 1 H) 2.40 (qd, J=5.65, 3.73 Hz, 1 H).

WORKUP

后处理

  1. temperaturewas refluxed for 2 hr
  2. additionThe reaction mixture was poured into a separatory funnel that
  3. customcontained crushed ice
  4. extractionextracted with ether (2×20 mL)
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated