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二甲基亚砜 → Dimethyl 1,1-difluoro-2-oxo-4,8,12-trimethyl-3,7,11-tridecatrienylphosphonate

HRID 2211368
笔记
打印预览

反应方程式

HRID 2211368 反应方程式
FC(F)(F)C(OC(=O)C(F)(F)F)=O.CS(C)=O.[F:18][C:19]([P:37](=[O:42])([O:40][CH3:41])[O:38][CH3:39])([F:36])[CH:20]([OH:35])[CH:21]=[C:22]([CH3:34])[CH2:23][CH2:24][CH:25]=[C:26]([CH3:33])[CH2:27][CH2:28][CH:29]=[C:30]([CH3:32])[CH3:31].C(N(CC)CC)C>ClCCl.O>[F:36][C:19]([P:37](=[O:42])([O:40][CH3:41])[O:38][CH3:39])([F:18])[C:20](=[O:35])[CH:21]=[C:22]([CH3:34])[CH2:23][CH2:24][CH:25]=[C:26]([CH3:33])[CH2:27][CH2:28][CH:29]=[C:30]([CH3:32])[CH3:31]
参与物实验过程后处理来源与证据反应笔记

参与物

7

反应物 4

HCID 679二甲基亚砜HCID 8471三乙胺HCID 9845三氟乙酸酐HCID 54561178Dimethyl 1,1-difluoro-2-hydroxy-4,8,12-trimethyl-3,7,11-tridecatrienylphosphonate

产物 1

HCID 53731468Dimethyl 1,1-difluoro-2-oxo-4,8,12-trimethyl-3,7,11-tridecatrienylphosphonate收率 69.2%

试剂、催化剂与溶剂 2

HCID 962
聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]
溶剂
HCID 6344二氯甲烷溶剂3 次

实验过程

Combine trifluoroacetic acid anhydride (1.30 mL, 0.0096 mol) with dichloromethane (20 mL) and cool to -60° C. Add dropwise a solution of dimethylsulfoxide (1.30 mL, 0.0183 mol) in dichloromethane (2 mL) while maintaining the temperature below -55° C. After addition is complete, stir for stir for 2 minutes. Add a solution of the dimethyl 1,1-difluoro-2-hydroxy-4,8,12-trimethyl-3,7,11-tridecatrienylphosphonate (1.60 g, 0.0042 mol) prepared in example 1 in dichloromethane (4 mL) and stir for 45 minutes. Cool the reaction to -78° C. and add triethylamine (3.0 mL, 0.021 mol) dropwise. Allow the reaction to warm to ambient temperature and stir for 45 minutes. Pour the reaction into water (100 mL). Extract this mixture with diethyl ether (400 mL). Dry the organic phase over anhydrous magnesium sulfate, filter and concentrate under vacuum. Purify the residue by flash chromatography (20% ethyl acetate/hexane, Rf = 0.18) to provide the title compound (1.1 g, 69%) as an oil.

后处理

  1. temperaturewhile maintaining the temperature below -55° C
  2. additionAfter addition
  3. stirringfor stir for 2 minutes
  4. stirringstir for 45 minutes
  5. temperatureCool
  6. customthe reaction to -78° C.
  7. customthe reaction
  8. stirringstir for 45 minutes
  9. additionPour
  10. extractionExtract this mixture with diethyl ether (400 mL)
  11. dry with materialDry the organic phase over anhydrous magnesium sulfate
  12. filtrationfilter
  13. concentrationconcentrate under vacuum
  14. customPurify the residue by flash chromatography (20% ethyl acetate/hexane, Rf = 0.18)

来源与证据

ORD记录
ord-42a8d50d435849b5aff05c5743671a69
来源数据集
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US05463181

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记