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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 54359738, 화합물

HRID 851324
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HRID 851324 반응식
[Na].C(OP([CH:10]([Cl:19])[C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)(=O)OCC)C.[CH3:20][C:21]([CH3:25])=[CH:22][CH:23]=O.O>C(O)C.O1CCCC1>[CH3:18][O:17][C:14]1[CH:13]=[CH:12][C:11]([C:10]([Cl:19])=[CH:23][CH:22]=[C:21]([CH3:25])[CH3:20])=[CH:16][CH:15]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 610203-Methyl-2-butenalHCID 5360545Sodium2회HCID 12874246HCID 12874246, 화합물

생성물 1

HCID 54359738HCID 54359738, 화합물수율 56.1%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 8028
Tetrahydrofuran
용매
3회

실험 절차

4.6 g (0.2 mol) of sodium were dissolved incrementally in 100 ml of dry ethanol. When all the sodium had dissolved, 100 ml of anhydrous tetrahydrofuran were added and 58.4 g (0.2 mol) of 4-methoxy-α-chloro-benzyl-phosphonic acid diethyl ester, dissolved in 50 ml of anhydrous tetrahydrofuran, were added dropwise at 0° C., while stirring. After stirring had been continued at 0°-10° C. for a further 1 hour, 16.8 g (0.2 mol) of β,β-dimethylacrolein, dissolved in 30 ml of anhydrous tetrahydrofuran, were added dropwise, while stirring. Stirring was then continued at room temperature for a further 12 hours. 600 ml of water were then added to the reaction mixture and the mixture was extracted twice with 300 ml of methylene chloride each time. The organic phase was separated off and dried over magnesium sulphate, the solvent was distilled off under a waterpump vacuum and the residue was distilled in vacuo. 25 g of 1-(4'-methoxyphenyl)-1-chloro-4,4-dimethyl-1,3-butadiene (isomer mixture) were obtained as a yellow oil which had a boiling point of 130°-145° C./2 mm Hg and partially crystallized after some time.

후처리

  1. additionwere added dropwise at 0° C.
  2. stirringAfter stirring
  3. additionwere added dropwise
  4. stirringwhile stirring
  5. stirringStirring
  6. waitwas then continued at room temperature for a further 12 hours
  7. extractionthe mixture was extracted twice with 300 ml of methylene chloride each time
  8. customThe organic phase was separated off
  9. dry with materialdried over magnesium sulphate
  10. distillationthe solvent was distilled off under a waterpump vacuum
  11. distillationthe residue was distilled in vacuo

출처 및 근거

ORD 기록
ord-4480576153254bc3a67258c4e8566494
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04384114

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