HRID1947505

反应详情

EQUATION

反应方程式

HRID 1947505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-(hydroxymethyl)furo[3,2-b]pyridin-6-ol (200 mg, 1.21 mmol), 2-chloro-thiazolo-[4,5-b]pyridine hydrochloride (300 mg, 1.45 mmol) and Cs2CO3 (800 mg, 2.46 mmol) was added DMF (12 mL). The suspension was stirred (rt, 16 h) and then poured into ice-cold sat'd. aq. NH4Cl. The resultant precipitate was filtered, rinsed with water and dried to provide the product as a beige solid (326 mg, 90%). MS (ESI): mass calcd. for C14H9N3O3S, 299.04; m/z found, 300.0 [M+H]+. 1H NMR (600 MHz, CD3OD): 8.63 (d, J=2.3, 1H), 8.49 (dd, J=4.9, 1.6, 1H), 8.36 (dd, J=8.0, 1.6, 1H), 8.23 (dd, J=2.3, 0.9, 1H), 7.37 (dd, J=8.0, 4.9, 1H), 6.95 (s, 1H), 4.76 (s, 2H).

WORKUP

后处理

  1. additionpoured into ice-cold sat'd
  2. filtrationThe resultant precipitate was filtered
  3. washrinsed with water
  4. customdried