2-[(2-Methyl-2-oxiranyl)methyl]phenol → (2-Methyl-2,3-dihydro-1-benzofuran-2-yl)methanol

HRID 648221노트

반응식

HRID 648221 반응식
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]1([CH3:12])[O:11][CH2:10]1>C(Cl)Cl>[OH:11][CH2:10][C:9]1([CH3:12])[CH2:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[O:1]1

참가 물질

3

반응물 1

HCID 118160462-[(2-Methyl-2-oxiranyl)methyl]phenol

생성물 1

HCID 20482667(2-Methyl-2,3-dihydro-1-benzofuran-2-yl)methanol수율 94.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1-(2-hydroxyphenyl)-2-methyl-2,3-epoxypropane (52.7 g) and silica (Kieselgel 60; 70-230 mesh) (150 g) in methylene chloride (300 ml) was stirred at room temperature for 24 hours. Removal of the solvent gave a residue of silica and absorbed product and this mixture was stirred with ethyl acetate for 3 hours. After filtration the ethyl acetate filtrate was dried and the solvent evaporated in vacuo to give the desired alcohol 49.6 g. This crude product was dissolved in methylene chloride and washed with 1 N aqueous sodium hydroxide solution, water and then dried. Removal of the solvent gave the alcohol as a yellow oil 37 g; I.R. νmax 3700-3200 cms-1.

후처리

  1. customRemoval of the solvent
  2. customgave a residue of silica
  3. customabsorbed product
  4. stirringthis mixture was stirred with ethyl acetate for 3 hours
  5. filtrationAfter filtration the ethyl acetate filtrate
  6. customwas dried
  7. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-34915629bf874e3488235eca6d307e01
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411908

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