反応 #3868

反応方程式

sodium borohydride

product

7-Methoxy-2,2-dimethyl-3-benzofuranone

→

7-Methoxy-3-hydroxy-2,2-dimethylbenzofuran

溶媒

methylene chloride

ethanol

反応条件

後処理

1. 1
   その他evaporated in vacuo
2. 2
   その他toluene, the layers are separated
3. 3
   洗浄the organic phase washed
4. 4
   その他dried
5. 5
   その他evaporated in vacuo
6. 6
   その他affording an oil which
7. 7
   その他dried
8. 8
   ろ過filtered
9. 9
   その他evaporated in vacuo
10. 10
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
11. 11
    その他chromatographed on silica gel affording the desired product as a white solid

実験手順

An aqueous solution of sodium borohydride (8.2 g, 50 ml) is added to a stirred solution of the product obtained in Step 3. (41.8 g) in ethanol (1 l) and the mixture refluxed for 3 hours and evaporated in vacuo. The residue is taken up in water and toluene, the layers are separated and the organic phase washed, dried and evaporated in vacuo affording an oil which is dissolved in methylene chloride, dried, filtered and evaporated in vacuo. The residue is dissolved in ethyl acetate and chromatographed on silica gel affording the desired product as a white solid.

出典