4-(Hydroxymethyl)cyclohexan-1-one → 4-(Hydroxymethyl)-1-methylcyclohexanol

HRID 1036042ノート

反応式

HRID 1036042 の反応式
[OH:1][CH2:2][CH:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.[CH3:10][Mg]Cl>O1CCCC1>[OH:1][CH2:2][CH:3]1[CH2:8][CH2:7][C:6]([CH3:10])([OH:9])[CH2:5][CH2:4]1

参加物

4

反応物 2

HCID 128928674-(Hydroxymethyl)cyclohexan-1-oneHCID 178418332HCID 178418332、化合物

生成物 1

HCID 232634014-(Hydroxymethyl)-1-methylcyclohexanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

4-(Hydroxymethyl)cyclohexanone (800 mg) in tetrahydrofuran (15 mL) was treated with 3 M methylmagnesium chloride in tetrahydrofuran (6.24 mL) at 0° C. The reaction was warmed to room temperature over 2 hours and quenched with methanol and water. The resulting mixture was concentrated and the residue was suspended in ethyl acetate. The precipitates were filtered off and the filtrate was concentrated. The residue was purified by chromatography, eluting with 0-100% ethyl acetate in hexane to provide the title compound.

後処理

  1. customquenched with methanol and water
  2. concentrationThe resulting mixture was concentrated
  3. filtrationThe precipitates were filtered off
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by chromatography
  6. washeluting with 0-100% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-6bf2dff1ce7f4dadbe2946d4672f69b0
出典データセット
uspto-grants-2013_10
特許番号
US08546399B2

反応ノート

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