HRID2074000
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
A mixture of the phenolic compound of step 6 above (4 g) and NaH (0.7 g) in DMF (50 ml) is stirred for 15 minutes. Dimethyl sulfate (2 g) is added and the mixture is stirred for 16 hours. The mixture is partitioned between CH2Cl2 and H2O, and the organic layer is separated and washed with H2O, dried (MgSO4) and evaporated. The solid residue is twice recrystallized from MeOH-H2O and chromatographed on silica gel affording the desired product which is used in the next step.
WORKUP
后处理
- stirringthe mixture is stirred for 16 hours
- customThe mixture is partitioned between CH2Cl2 and H2O
- customthe organic layer is separated
- washwashed with H2O
- dry with materialdried (MgSO4)
- customevaporated
- customThe solid residue is twice recrystallized from MeOH-H2O
- customchromatographed on silica gel affording the desired product which