Iodoethane → 4-Hydroxy-2,2-dimethylbutyric acid ethyl ester

HRID 409479

反応式

HRID 409479 の反応式
[OH:1][CH2:2][CH2:3][C:4]([CH3:9])([CH3:8])[C:5]([O-:7])=[O:6].[K+].[CH2:11](I)[CH3:12]>CN(C=O)C>[CH2:11]([O:6][C:5](=[O:7])[C:4]([CH3:9])([CH3:8])[CH2:3][CH2:2][OH:1])[CH3:12]

参加物

4

反応物 2

HCID 6340IodoethaneHCID 23712640Potassium 4-hydroxy-2,2-dimethylbutyrate

生成物 1

HCID 596143744-Hydroxy-2,2-dimethylbutyric acid ethyl ester収率 169%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of potassium 4-hydroxy-2,2-dimethylbutyrate (1.92 mmol; 327 mg) in DMF (6 mL) is added ethyl iodide (2.30 mmol; 359 mg). The reaction mixture is stirred for 2 hours, and quenched with saturated ammonium chloride solution. The product is extracted three times with EtOAc. The combined organic layer is washed with aqueous 0.1 M HCl then brine, dried over Na2SO4, filtered, concentrated under reduced pressure to give 4-Hydroxy-2,2-dimethylbutyric acid ethyl ester (520 mg) contaminated with DMF.

後処理

  1. customquenched with saturated ammonium chloride solution
  2. extractionThe product is extracted three times with EtOAc
  3. washThe combined organic layer is washed with aqueous 0.1 M HCl
  4. dry with materialbrine, dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-de5cbd37edc14a33bced3ed4b90033ff
出典データセット
uspto-grants-2014_06
特許番号
US08759365B2

関連ノート

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