HRID1392559
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
PROCEDURE
实验过程
5-(2,6-Dibromo-3-methyl-4-nitrophenoxy)-2-hydroxy-3-isopropylbenzaldehyde of Part 8D (100 mg, 0.21 mmol) and NaBH4 (9.0 mg, 0.23 mmol) was dissolved in a mixture of EtOH and THF (3 mL, 2:1) at room temperature. After 1.5 hours of stirring at room temperature, the reaction mixture was concentrated and the residue suspended in CHCl3. The suspension was washed with 1N HCl and the two phases were separated with a phase separator (IST) before concentration of the organic phase. The residue was purified on column (silica gel, gradient elution: n-heptane/EtOAc from 1:0 to 7:3) to give 85 mg (85%) of 4-(2,6-dibromo-3-methyl-4-nitrophenoxy)-2-hydroxymethyl-6-isopropylphenol as a light yellow foam.
WORKUP
后处理
- concentrationthe reaction mixture was concentrated
- washThe suspension was washed with 1N HCl
- customthe two phases were separated with a phase separator (IST) before concentration of the organic phase
- customThe residue was purified on column (silica gel, gradient elution: n-heptane/EtOAc from 1:0 to 7:3)