Sodium Iodide → Ethyl 3-Hydroxybutyrate

HRID 327865

반응식

HRID 327865 반응식
[Na+].[I-].[C:3]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:4][C:5]([CH3:7])=[O:6].[H][H]>O>[OH:6][CH:5]([CH3:7])[CH2:4][C:3]([O:9][CH2:10][CH3:11])=[O:8]

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 8868Ethyl AcetoacetateHCID 178418361HCID 178418361, 화합물3회

생성물 1

HCID 62572Ethyl 3-Hydroxybutyrate수율 63%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
65 °C

실험 절차

Under a nitrogen gas atmosphere, 0.0096 g (7.3×10-6 mol) of [RuI(p-Cymene)((+)-SO3Na-BINAP)]I, 0.1164 g (7.8×10-4 mol) of NaI, 1 ml (7.5×10-3 mol) of ethyl acetoacetate, and 1.5 ml of water were charged in a 100 milli-liter autoclave. After displacing the inside atmosphere of the autoclave with a hydrogen gas, the autoclave was pressed at a hydrogen pressure of 50 kg/cm2 and the mixture was stirred for 40 hours at 65° C. After the reaction was over, the hydrogen gas was removed, and after added thereto 100 ml of water and 100 ml of ether, the ether extraction was carried out. The ether extract was recovered, dried with anhydrous sodium sulfate, and further ether was distilled off to provide 0.62 g (percent yield 63%) of ethyl 3-hydroxybutyrate. By the analysis of gas chromatography (PEG-HT), the conversion ratio was determined to be 99%.

후처리

  1. customwas removed
  2. additionafter added
  3. extraction100 ml of water and 100 ml of ether, the ether extraction
  4. extractionThe ether extract
  5. customwas recovered
  6. dry with materialdried with anhydrous sodium sulfate, and further ether
  7. distillationwas distilled off

출처 및 근거

ORD 기록
ord-5ab3e6632dd54e23a7176b1dc9864c6e
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05274146

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