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Diethyl Ether → HCID 20343275, 화합물

HRID 2050079
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HRID 2050079 반응식
[C-:1]#[N:2].[K+].[F:4][C:5]([F:18])([O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14]Br)=[CH:12][CH:11]=1)[CH:6]([F:8])[F:7].CCOCC>O>[F:4][C:5]([F:18])([O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14][C:1]#[N:2])=[CH:12][CH:11]=1)[CH:6]([F:8])[F:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 9032Potassium CyanideHCID 222617841-(Bromomethyl)-4-(1,1,2,2-tetrafluoroethoxy)benzene

생성물 1

HCID 20343275HCID 20343275, 화합물수율 87.9%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Over a period of 40 minutes, a hot solution of 75.1 g (1.15 mol) of potassium cyanide in 140 ml of water is added to a mechanically stirred 75° C. solution of 160.99 g (0.561 mol) of p-(1,1,2,2-tetrafluoroethoxy)benzyl bromide and 500 ml of anhydrous 2B alcohol. The resulting mixture is refluxed for 1.75 hours. After sitting overnight the reaction mixture is poured into 500 ml of cold water and 400 ml of ether. The combined ether solutions are washed twice with 500 ml of water, dried with sodium sulfate, filtered, and then evaporated on a rotary evaporator to give 114.95 g of an oil. A vacuum distillation of this oil gives, as one distillation fraction, 37.10 g (28%) of the nitrile, boiling point 85° C. to 100° C. at 0.29 mm Hg.

후처리

  1. temperatureThe resulting mixture is refluxed for 1.75 hours
  2. waitAfter sitting overnight
  3. washThe combined ether solutions are washed twice with 500 ml of water
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. customevaporated on a rotary evaporator

출처 및 근거

ORD 기록
ord-4ae9b7b057e247bfa6cd158891346bc5
출처 데이터셋
uspto-grants-1980_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04199595

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