HRID1190273

反应详情

EQUATION

反应方程式

HRID 1190273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(4-isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-8-carboxylic acid methyl ester (620 mg, 1.67 mmol) in THF (12 mL) at 0° C. was added LiAlH4 (152 mg, 4.02 mmol). The reaction mixture was stirred for 4 hours at RT before being quenched with H2O (0.15 mL), 15% NaOH(aq) (0.15 mL) and H2O (0.45 mL). The precipitate was removed by filtration, washing with methanol/DCM, and then the filtrate was concentrated in vacuo to yield the title compound as an orange solid (563 mg, 98%). LCMS: RT=3.71 min, [M+H]+=343

WORKUP

后处理

  1. custombefore being quenched with H2O (0.15 mL), 15% NaOH(aq) (0.15 mL) and H2O (0.45 mL)
  2. customThe precipitate was removed by filtration
  3. washwashing with methanol/DCM
  4. concentrationthe filtrate was concentrated in vacuo