HRID1159368

反应详情

EQUATION

反应方程式

HRID 1159368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Intermediate 5, tert-Butyl [(cis-3-hydroxycyclobutyl)methyl]methylcarbamate (22.6 g, 105 mmol) and triethylamine (36 mL, 250 mmol) were dissolved in CH2Cl2 (50 mL). MsCl (9.75 mL, 126 mmol) was added dropwise at −20° C. under stirring in argon. The temperature was brought to ambient within 1 h. Water (100 mL) was added, and the layers were separated. The organic one was washed with water, brine, dried with Na2SO4, and evaporated. The title compound (29 g, 96%) was obtained as a yellow oil. This crude product was used for the next stage without additional purification. 1H NMR-data (DMSO-d6): 4.76-4.88 (m, 1H); 3.23 (d, 2H, CH2, J=6.6 Hz); 3.12 (s, 3H, MS); 2.76 (s, 3H, NCH3); 2.38-2.48 (m, 2H); 2.00-2.12 (m, 1H); 1.86-97 (m, 2H); 1.38 (s, 9H, Boc).

WORKUP

后处理

  1. customthe layers were separated
  2. washThe organic one was washed with water, brine
  3. dry with materialdried with Na2SO4
  4. customevaporated