HRID527726
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
3-(1,1-dimethylethyl)-4-hydroxybenzaldehyde (Reference Intermediate R9, 550 mg) and hydroxylamine hydrochloride (322 mg, 4.63 mmol) were stirred in 8.0 mL of acetic acid at reflux for 1 h. After cooling down to 0° C., the mixture was poured into Et2O and washed once with water and once with NaOH (5% aqueous solution). The collected aqueous phases were extracted with Et2O (two times) and the combined organic phases were dried over Na2SO4, filtered, evaporated and triturated with pentane affording 540 mg of the title compound.
WORKUP
后处理
- temperatureat reflux for 1 h
- washwashed once with water and once with NaOH (5% aqueous solution)
- extractionThe collected aqueous phases were extracted with Et2O (two times)
- dry with materialthe combined organic phases were dried over Na2SO4
- filtrationfiltered
- customevaporated
- customtriturated with pentane affording 540 mg of the title compound