HRID499474

反应详情

EQUATION

反应方程式

HRID 499474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[6-(Aminomethyl)-2-pyridyl]-4H-1,3-benzothiazine-4-one trifluoroacetic acid salt (350 mg, 0.91 mmol) was dissolved in pyridine (10 ml), and methanesulfonyl chloride (576 mg, 5.04 mmol) was added thereto. The reaction mixture was stirred at room temperature for 3 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethyl acetate (1:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (228 mg, 68%) as pale yellow crystals.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. washThe fractions eluted with hexane-ethyl acetate (1:1
  3. customv/v) were collected
  4. concentrationconcentrated
  5. customrecrystallized from hexane-tetrahydrofuran