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

HRID 1604535ノート

反応式

HRID 1604535 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-835531211c48453f945a09491a20612c
出典データセット
uspto-grants-1999_11
特許番号
US05994368

反応ノート

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