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Hydrochloric Acid → HCID 11321150, 화합물

HRID 1655764
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HRID 1655764 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[C:14](O)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>CCOCC>[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[CH2:14][OH:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7233172(S)-3-methyl-2-phenylbutanoic acidHCID 21226445Aluminium lithium hydride

생성물 1

HCID 11321150HCID 11321150, 화합물수율 105.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A suspension of 19.5, g (0.51 mol) of lithium aluminium hydride in 750 ml of absolute ether was heated to reflux. Within 4 hours there was added, dropwise, a solution of 54.5 g (0.307 mol) of (S)-(+)-2-phenyl 3-methylbutyric acid in 250 ml of absolute ether. After heating to reflux for a further 2 hours, the suspension was treated carefully with 1N hydrochloric acid and the ether phase was washed with water, dilute sodium bicarbonate solution, and once more with water. After drying the organic phase over sodium sulfate and evaporation under reduced pressure, there were obtained 53.1 g of (S)-(+)-2-phenyl-3-methylbutanol as a thick oil which was used directly in the next step.

후처리

  1. temperaturewas heated to reflux
  2. additionWithin 4 hours there was added
  3. temperatureAfter heating
  4. temperatureto reflux for a further 2 hours
  5. washthe ether phase was washed with water, dilute sodium bicarbonate solution
  6. customAfter drying the organic phase
  7. customover sodium sulfate and evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-03e11201694046bcbabb459347e33315
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250517

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