O-Cresol → 1-(Methoxymethoxy)-2-methylbenzene

HRID 1669460

반응식

HRID 1669460 반응식
[H-].[Na+].[C:3]1([CH3:10])[C:8]([OH:9])=[CH:7][CH:6]=[CH:5][CH:4]=1.C[CH2:12][O:13][CH2:14]C.C(Cl)OC>CCOCC.CN(C=O)C.O>[CH3:12][O:13][CH2:14][O:9][C:8]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:10]

참가 물질

7

반응물 4

HCID 335O-CresolHCID 3283Diethyl Ether2회HCID 7864Chloromethyl Methyl EtherHCID 24758Sodium hydride

생성물 1

HCID 38393511-(Methoxymethoxy)-2-methylbenzene

시약·촉매·용매 2

HCID 962Water용매HCID 19966313DMF ether용매

실험 절차

To a suspension of NaH (60% dispersion in mineral oil; 1.2 eq) in Et2O/DMF (5:1, 0.2M) a solution of o-cresol in Et2O (1 eq, 2M) was added dropwise over 15 min. A solution of MOMCl in Et2O (1.1 eq, 2M) was added and the mixture was stirred for 30 min then poured into H2O and extracted with Et2O. The combined organic extracts were washed with 1N NaOH, H2O and brine, dried over Na2SO4, filtered and evaporated in vacuo to give the title compound. The product was used in the next step without further purification.

후처리

  1. additionwas added dropwise over 15 min
  2. extractionextracted with Et2O
  3. washThe combined organic extracts were washed with 1N NaOH, H2O and brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-20b43335f7ed4d1abe3450533abe617c
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989438B2

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