HRID366431

反应详情

EQUATION

反应方程式

HRID 366431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

7-Methoxy-2-methyl-benzothiazole (400 mg, 2.23 mmol) was mechanically mixed with solid pyridine hydrochloride (6.00 g, 52 mmol) and then heated to 160-170° C. in a sealed vessel for 16 hours. Water (40 mL) was added to the warm mixture, the pH was adjusted to neutrality with NaHCO3 and the mixture was extracted with 1:1 CHCl2 /CHCl3 (4×10 mL). The pooled organic extracts were dried over MgSO4, filtered, and concentrated in vacuo to provide 2-methyl-benzothiazol-7-ol as a waxy yellow solid. (260 mg; GC-MS m/z 165).

WORKUP

后处理

  1. extractionthe mixture was extracted with 1:1 CHCl2 /CHCl3 (4×10 mL)
  2. dry with materialThe pooled organic extracts were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo