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Dimethylformamide → HCID 54049871, 화합물

HRID 2164182
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HRID 2164182 반응식
[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]
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참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 66113Methyl diethylphosphonoacetateHCID 54017105HCID 54017105, 화합물

생성물 1

HCID 54049871HCID 54049871, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a874b5230b94ef291be9b77086adcb3
출처 데이터셋
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04137273

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