Water → HCID 58097238、化合物

HRID 1630717ノート

反応式

HRID 1630717 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[CH:5][CH:4]=1.ClC[C@@H:13]1[CH2:17][O:16][C:15]([CH3:19])([CH3:18])[O:14]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH3:18][C:15]1([CH3:19])[O:16][C@H:17]([CH2:1][O:2][C:3]2[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[CH:5][CH:4]=2)[CH2:13][O:14]1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 312444-MethoxybenzaldehydeHCID 6930483(S)-4-Chloromethyl-2,2-dimethyl-1,3-dioxolane

生成物 1

HCID 58097238HCID 58097238、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2 g (16.38 mmol) of p-methoxybenzaldehyde together with 3.7 g (24.57 mmol) of (4S)-4-(chloromethyl)-2,2-dimethyl-1,3-dioxolane and 15.8 g (114.64 mmol) of potassium carbonate are stirred in 10 ml of DMF at 130° C. overnight. The mixture is then added to water and extracted with methylene chloride. The organic phase is washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated. The residue is purified on a silica gel column (mobile phase: cyclohexane/ethyl acetate 5:1). This gives 2.42 g (61% of theory) of the target compound.

後処理

  1. extractionextracted with methylene chloride
  2. washThe organic phase is washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated
  5. customThe residue is purified on a silica gel column (mobile phase: cyclohexane/ethyl acetate 5:1)

出典と根拠

ORDレコード
ord-038ed0892cca4d9698a4a8898026f65f
出典データセット
uspto-grants-2014_07
特許番号
US08791146B2

反応ノート

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