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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Diethyl Ether → HCID 12786232、化合物

HRID 126722
ノート
印刷プレビュー

反応式

HRID 126722 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 3283Diethyl Ether2 回HCID 7842Propargyl bromideHCID 619224-(Methylthio)-2-butanoneHCID 5462224Magnesium

生成物 1

HCID 12786232HCID 12786232、化合物

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-503ffd60b4c04ddb8b1ce060ccb8fec5
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04254036

反応ノート

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