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Diethyl Ether → HCID 12786232, 화합물

HRID 848912
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HRID 848912 반응식
[Mg].[CH2:2](Br)[C:3]#C.[CH3:6][S:7][CH2:8][CH2:9][C:10](=[O:12])[CH3:11].[CH3:13]COCC>>[OH:12][C:10]([CH3:13])([CH2:9][CH2:8][S:7][CH3:6])[CH2:11][C:2]#[CH:3]
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참가 물질

5

반응물 4

HCID 3283Diethyl Ether2회HCID 7842Propargyl bromideHCID 619224-(Methylthio)-2-butanoneHCID 5462224Magnesium

생성물 1

HCID 12786232HCID 12786232, 화합물

실험 절차

To a stirred mixture of 6.6 g. (0.275 moles) of magnesium and 116 mg. of mercuric chloride in 35 ml. of ether is added, dropwise under argon atmosphere, 35.2 g. of propargyl bromide (80% solution in toluene) and 25 g. (0.21 moles) of methylmercaptobutane-3-one [D. B. Reisner, J. Am. Chem. Soc., 78, 2132 (1956) in 100 ml. of ether at a rate to maintain gentle refluxing. After stirring at the reflux temperature for 35 minutes, the cooled mixture is quenched by dropwise addition of 140 ml. of saturated ammonium chloride solution. The ether phase is separated, washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate and taken to dryness. Distillation of the residual oil provides 27.4 g. (82%) of product as a colorless oil; b.p 114°-115° C. (7-8 mm.).

후처리

  1. additionTo a stirred mixture of 6.6 g
  2. customthe cooled mixture is quenched by dropwise addition of 140 ml
  3. customThe ether phase is separated
  4. washwashed with saturated sodium chloride solution
  5. dry with materialdried with anhydrous magnesium sulfate
  6. distillationDistillation of the residual oil
  7. customprovides 27.4 g
  8. customb.p 114°-115° C. (7-8 mm.)

출처 및 근거

ORD 기록
ord-1d3e084af94644a18bbf7aba4a794638
출처 데이터셋
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04297516

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