HRID1099438

反应详情

EQUATION

反应方程式

HRID 1099438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 6-[(3,3,3-trifluoropropyl)carbamoyl]nicotinate (0.265 g, 0.96 mmol), sodium hydroxide (9.60 ml, 9.60 mmol), and ethanol (10 mL) was heated to 50° C. for 3.5 h. The volatiles were removed in vacuo. The residue was suspended in water (20 mL) and insoluble material was filtered off. The filtrate was cooled on ice and 6 M hydrochloric acid was added while stirring until an acidic pH was reached. The precipitate was filtered off, washed with ice-water and dried in vacuo to yield 78 mg (31%); MS (APPI/APCI) m/z 263[M+H+].

WORKUP

后处理

  1. customThe volatiles were removed in vacuo
  2. filtrationinsoluble material was filtered off
  3. temperatureThe filtrate was cooled on ice and 6 M hydrochloric acid
  4. additionwas added
  5. filtrationThe precipitate was filtered off
  6. washwashed with ice-water
  7. customdried in vacuo
  8. customto yield 78 mg (31%)