반응 #481827

반응 방정식

alcohol

2,3-Dihydro-1,4-benzodioxin-6-ol

NaH

iodomethane

→

6-Methoxy-2,3-dihydro-1,4-benzodioxin

용매

DMF

반응 조건

후처리

1. 1
   기타the DMF is then evaporated
2. 2
   세척Washing with ethyl acetate and with water
3. 3
   기타the two phases are separated
4. 4
   건조The combined organic phases are dried over MgSO4
5. 5
   기타the solvent is evaporated
6. 6
   기타The oil obtained
7. 7
   기타is purified on a silica column (eluant: PE/AcOEt 8/2), which
8. 8
   기타to be obtained

실험 절차

3 g (18.05 mmol) of the alcohol obtained in Step A are dissolved in 10 ml of DMF in a flask. 2 eq. of NaH (60% in oil) are added slowly and allowed to act for 30 minutes under an inert atmosphere. 2 eq. of iodomethane are then added. The mixture is stirred for 2 hours; the DMF is then evaporated. Washing with ethyl acetate and with water is carried out and the two phases are separated. The combined organic phases are dried over MgSO4 and the solvent is evaporated. The oil obtained is purified on a silica column (eluant: PE/AcOEt 8/2), which allows the pure title product to be obtained.

출처