HRID1775470

反应详情

EQUATION

反应方程式

HRID 1775470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-{4-chloro-6-[(3,3-difluorocyclobutyl)amino]-2-(methylsulfanyl)pyrimidin-5-yl}ethanol (714 mg, 2.31 mmol) in DCM (38.5 mL) was added TEA (1.12 mL, 8.06 mmol), methanesulfonyl chloride (0.455 mL, 5.76 mmol) and DMAP (17 mg, 0.138 mmol) at 0° C. The mixture was stirred at 0° C. for 1 h and at room temperature for 1 h. The reaction mixture was washed with water (3×), and the organic layer was dried (Na2SO4) and concentrated under reduced pressure to give 925 mg (>99%) of the title compound as a yellow solid. This material was used in the next step without further purification. 1H NMR (400 MHz, DMSO-d6) δ 7.67 (d, J=5.7 Hz, 1 H), 4.40-4.29 (m, 1 H), 4.26 (t, J=6.8 Hz, 2 H), 3.14 (s, 3 H), 3.05 (t, J=6.8 Hz, 2 H), 3.02-2.89 (m, 2 H), 2.85-2.68 (m, 2 H), 2.44 (s, 3 H). m/z (APCI+) for C12H16ClF2N3O3S2 388.0 (M+H)+.

WORKUP

后处理

  1. washThe reaction mixture was washed with water (3×)
  2. dry with materialthe organic layer was dried (Na2SO4)
  3. concentrationconcentrated under reduced pressure