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

HRID 409479

반응식

HRID 409479 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 596143744-Hydroxy-2,2-dimethylbutyric acid ethyl ester수율 169%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-de5cbd37edc14a33bced3ed4b90033ff
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759365B2

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