Water → 2,6-Dichloro-3-(methoxymethoxy)benzyl alcohol

HRID 1604535노트

반응식

HRID 1604535 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[C:18]([O:19][CH2:20][O:21][CH3:22])=[CH:17][CH:16]=[C:15]([Cl:23])[C:9]=1[C:10](OCC)=[O:11].O>O1CCCC1>[Cl:7][C:8]1[C:18]([O:19][CH2:20][O:21][CH3:22])=[CH:17][CH:16]=[C:15]([Cl:23])[C:9]=1[CH2:10][OH:11]

참가 물질

5

반응물 3

HCID 962WaterHCID 19603256Ethyl 2,6-dichloro-3-(methoxymethoxy)benzoateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 536407392,6-Dichloro-3-(methoxymethoxy)benzyl alcohol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of lithium aluminum hydride (347 mg) in tetrahydrofuran was dropwise added a solution of ethyl 2,6-dichloro-3-(methoxymethoxy)benzoate (2.55 g) in tetrahydrofuran at 0° C. under nitrogen atmosphere, and the mixture was stirred for 30 minutes at the same temperature and for 18 hour at ambient temperature. Water was dropwise added thereto at 0° C., and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash chromatography (n-hexane:ethyl acetate=6:1, V/V) to give 2,6-dichloro-3-(methoxymethoxy)benzyl alcohol.

후처리

  1. extractionat 0° C., and the mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was purified by flash chromatography (n-hexane:ethyl acetate=6:1, V/V)

출처 및 근거

ORD 기록
ord-835531211c48453f945a09491a20612c
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05994368

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