Methanol → HCID 19421622、化合物

HRID 1613314ノート

反応式

HRID 1613314 の反応式
[C:1]1(/[C:7](/[C:13]#[C:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:8]\[C:9]([O:11]C)=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[OH-].[Na+]>O1CCCC1>[C:1]1(/[C:7](/[C:13]#[C:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:8]\[C:9]([OH:11])=[O:10])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 86746608HCID 86746608、化合物

生成物 1

HCID 19421622HCID 19421622、化合物収率 96.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 1.000 g of methyl (E)-3,5-diphenylpent-2-en-4-ynoate (prepared as described in Preparation 104), 15 ml of methanol, 7.5 ml of tetrahydrofuran and 15 ml of a 10% w/v aqueous solution of sodium hydroxide was stirred for 18 hours at room temperature. At the end of this time, the solvent was distilled off under reduced pressure. The resulting residue was diluted with water and extracted twice with diethyl ether. The ethereal extracts were washed with water, dried over anhydrous sodium sulfate and condensed by evaporation under reduced pressure, to give 0.912 g of the title compound, melting at 124°-126° C. (after recrystallisation from a mixture of methylene chloride and hexane).

後処理

  1. distillationAt the end of this time, the solvent was distilled off under reduced pressure
  2. additionThe resulting residue was diluted with water
  3. extractionextracted twice with diethyl ether
  4. washThe ethereal extracts were washed with water
  5. dry with materialdried over anhydrous sodium sulfate and condensed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-b2e5849f62454351b99b9688d0102007
出典データセット
uspto-grants-1993_03
特許番号
US05192766

反応ノート

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