HRID1096844

反应详情

EQUATION

反应方程式

HRID 1096844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Aq. 1M NaOH (1.0 mL) was added to a sol. of the compound C5 (50 mg, 0.090 mmol) in EtOH (1.0 mL). The resulting mixture was stirred at 70° C. for 1 h, cooled to rt and the solvent removed in vacuo. The crude mixture was partitioned between Et2O and aq. sat. NH4Cl. The aq. layer was extracted once more with Et2O, then acidified to pH= 4-5, and extracted again with Et2O. The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to yield the title compound (26.4 mg, 56%), which was not further purified. LC-MS: tR=0.82 min, ES+: 526.41.

WORKUP

后处理

  1. temperaturecooled to rt
  2. customthe solvent removed in vacuo
  3. customThe crude mixture was partitioned between Et2O and aq. sat. NH4Cl
  4. extractionThe aq. layer was extracted once more with Et2O
  5. extractionextracted again with Et2O
  6. dry with materialextracts were dried over MgSO4
  7. filtrationfiltered
  8. customthe solvents were removed under reduced pressure