Chloromethyl Methyl Ether → 2-Benzyl-1-methoxymethyloxy-4-iodobenzene

HRID 2216349

반응식

HRID 2216349 반응식
[CH2:1]([C:8]1[CH:13]=[C:12]([I:14])[CH:11]=[CH:10][C:9]=1[OH:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:16][O:17][CH2:18]Cl.O1CCCC1.[H-].[Na+]>O>[CH2:1]([C:8]1[CH:13]=[C:12]([I:14])[CH:11]=[CH:10][C:9]=1[O:15][CH2:16][O:17][CH3:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 7864Chloromethyl Methyl EtherHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 219422992-Benzyl-4-iodophenol

생성물 1

HCID 219423042-Benzyl-1-methoxymethyloxy-4-iodobenzene

시약·촉매·용매 1

HCID 962Water용매

실험 절차

10.1 g of 2-benzyl-1-hydroxy-4-iodobenzene and 3 ml of chloromethyl methyl ether were added to 100 ml of tetrahydrofuran and while stirring on an ice bath, 1.45 g of 60% (oily) sodium hydride was added dropwise to the mixture. After stirring for 2 hours, water was added to the reaction mixture, which then was extracted with ethyl acetate, washed with saturated brine and thereafter dried over anhydrous magnesium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography with 10% ethyl acetate/hexane, to give 8.7 g of the title compound.

후처리

  1. stirringAfter stirring for 2 hours
  2. extractionthen was extracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed
  6. customthe residue was purified by silica gel column chromatography with 10% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-d1ca98b4f2744c7490f5e8fb06c967dd
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112593B2

연결된 노트

불러오는 중…