HRID345776

反应详情

EQUATION

反应方程式

HRID 345776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1 M solution of BBr3 in CH2Cl2 (23 mL, 0.022 mol) was cooled to -80° C. in a dry ice/acetone bath under a N2 atmosphere. A suspension of 6-ethoxy-2-benzothiazolesulfonamide (0.5 g, 0.002 mol) in 75 mL of CH2Cl2 was added slowly to the cooled BBR3 solution The reaction was removed from the cooling bath and stirred at room temperature for 15 hours. It was poured into ice-water, stirred for 30 min, and filtered to Yield 0.35 g of product (73.8%). The product was purified by recrystallization from MeOH/H2O; mp 209°-212° C.; M/S m/e 230 (M,calcd 230).

WORKUP

后处理

  1. additionwas added slowly to the cooled BBR3 solution The reaction
  2. customwas removed from the cooling bath
  3. additionIt was poured into ice-water
  4. stirringstirred for 30 min
  5. filtrationfiltered