HRID1452760

反应详情

EQUATION

反应方程式

HRID 1452760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 5-morpholin-4-ylmethyl-furan-2-carboxylic acid hydrochloride in thionyl chloride with 2 drops of DMF was refluxed under N2 for 3 hours, then cooled to room temperature. Dry CH2Cl2 was added and solvents were evaporated in vacuo. The residue was triturated with dry CH2Cl2, and the resulting solid was filtered, washed with dry CH2Cl2 and dried in vacuo to give 373 mg (83% yield) of 5-morpholin-4-ylmethyl-furan-2-carbonyl chloride hydrochloride as a white solid. 1H-NMR (d6-DMSO) δ: 11.54 (broad s, 1H), 7.26 (d, 1H), 6.92 (d, 1H), 4.49 (s, 2H), 3.94 (m, 2H), 3.74 (m, 2H), 3.28 (m, 2H), 3.09 (broad s, 2H).

WORKUP

后处理

  1. temperaturewas refluxed under N2 for 3 hours
  2. customsolvents were evaporated in vacuo
  3. customThe residue was triturated with dry CH2Cl2
  4. filtrationthe resulting solid was filtered
  5. washwashed with dry CH2Cl2
  6. customdried in vacuo