HRID453383

反应详情

EQUATION

反应方程式

HRID 453383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To methyl 5-((2-cyclopentylethyl)carbamoyl)-2-methylbenzoate (1.2 g, 4.3 mmol) dissolved in THF (15 mL) was added a solution of LiOH, monohydrate (0.27 g, 6.4 mmol) in water (15 mL). The reaction mixture was stirred at RT for 18 h. THF was removed, the residue was extracted with ether (5 mL) and the layers were separated. To the aqueous layer was added 2N HCl until pH 4-5 (a lot of precipitate formed). The solid was collected by filtration, washed with water, dried to give 5-((2-cyclopentylethyl)carbamoyl)-2-methylbenzoic acid as a white solid. MS (ESI, pos. ion) m/z: 276.2 (M+1).

WORKUP

后处理

  1. customTHF was removed
  2. extractionthe residue was extracted with ether (5 mL)
  3. customthe layers were separated
  4. additionTo the aqueous layer was added 2N HCl until pH 4-5 (a lot of precipitate
  5. customformed)
  6. filtrationThe solid was collected by filtration
  7. washwashed with water
  8. customdried