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Dimethylformamide → HCID 54049871、化合物

HRID 2164182
ノート
印刷プレビュー

反応式

HRID 2164182 の反応式
[C:1]([CH2:5]P(=O)(OCC)OCC)([O:3][CH3:4])=[O:2].CN(C)C=O.[H-].[Na+].[CH3:21][C:22]([CH2:30][CH3:31])=[CH:23][CH2:24][CH2:25][CH2:26][C:27](=O)[CH3:28]>O>[CH3:28][C:27]([CH2:26][CH2:25][CH2:24][CH:23]=[C:22]([CH3:21])[CH2:30][CH3:31])=[CH:5][C:1]([O:3][CH3:4])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 66113Methyl diethylphosphonoacetateHCID 54017105HCID 54017105、化合物

生成物 1

HCID 54049871HCID 54049871、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 11.2 g. of diethyl carbomethoxymethylphosphonate in 100 ml. of dimethylformamide is treated with 2.4 g. of sodium hydride. The mixture is stirred until the evolution of gas ceases and then 10 g. of 7-methyl-6-nonen-2-one is added slowly with stirring, maintaining temperature below 30°. The mixture is stirred for about one hour, then diluted with water and then extracted with ether. The ethereal phase is washed with water, dried over sodium sulfate and evaporated under reduced pressure to yield methyl 3,8-dimethyldeca-2,7-dienoate as a mixture of isomers (trans,cis; trans,trans; cis,cis and cis,trans) which are separated by chromatography.

後処理

  1. additionA mixture of 11.2 g
  2. stirringwith stirring
  3. temperaturemaintaining temperature below 30°
  4. stirringThe mixture is stirred for about one hour
  5. extractionextracted with ether
  6. washThe ethereal phase is washed with water
  7. dry with materialdried over sodium sulfate
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-6a874b5230b94ef291be9b77086adcb3
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04137273

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート