HRID2204185

反应详情

EQUATION

反应方程式

HRID 2204185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

MgSO4 (4.82 g, 40.0 mmol), DCM (40 mL), and H2SO4 (533 μL, 10.0 mmol) were combined at 0° C. and the mixture was allowed to stir for 30 minutes at 0° C. 4-Bromo-3-methoxy-benzoic acid (2.31 g, 10.0 mmol) and 2-methylpropan-2-ol (4.78 mL, 50.0 mmol) were added and the mixture was allowed to stir at rt overnight. The mixture was filtered to remove the MgSO4 and the filtrate was washed with 1N NaOH. The layers were separated and the organic layer was dried over sodium sulfate and the solvent was removed to yield 400 mg of tert-butyl 4-bromo-3-methoxybenzoate. ESI-MS m/z calc. 286.0, found 287.0 (M+1)+; Retention time: 3.11 minutes (4 min run).

WORKUP

后处理

  1. customwere combined at 0° C.
  2. stirringto stir at rt overnight
  3. filtrationThe mixture was filtered
  4. customto remove the MgSO4
  5. washthe filtrate was washed with 1N NaOH
  6. customThe layers were separated
  7. dry with materialthe organic layer was dried over sodium sulfate
  8. customthe solvent was removed