Carbon Tetrachloride → alpha,alpha'-Dichloro-2,5-difluoro-para-xylene

HRID 1391074노트

반응식

HRID 1391074 반응식
C(N(CC)CC)C.P(Cl)(Cl)(Cl)(Cl)Cl.P(Cl)(Cl)([Cl:16])=O.O[CH2:20][C:21]1[CH:26]=[C:25]([F:27])[C:24](CO)=[CH:23][C:22]=1[F:30].Cl[C:32]([Cl:35])(Cl)Cl>C1C=CC=CC=1>[Cl:16][CH2:20][C:21]1[CH:26]=[C:25]([F:27])[C:24]([CH2:32][Cl:35])=[CH:23][C:22]=1[F:30]

참가 물질

7

반응물 5

HCID 5943Carbon TetrachlorideHCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 226301921,4-Benzenedimethanol, 2,5-difluoro-

생성물 1

HCID 21332303alpha,alpha'-Dichloro-2,5-difluoro-para-xylene

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
70 °C

실험 절차

While cooling with ice, 3 g of triethylamine are added to a mixture of 25 g of phosphorus pentachloride and 25 g of phosphorus oxychloride. After that, a solution of 2.2 g of α,α'-dihydroxy-2,5-difluoro-para-xylene in 10 ml of tetrachloromethane are added. The batch is heated at 70° C. for two hours. It is then cooled, poured onto ice, and dissolved in benzene. The benzene solution is washed with aqueous sodium carbonate solution, then dried with calcium chloride. The solvent is evaporated and the residue recrystallized several times from aqueous methanol. There are obtained 1.85 g of fine colorless needles melting at 62.5 - 64.5° C.

후처리

  1. temperatureIt is then cooled
  2. additionpoured onto ice
  3. washThe benzene solution is washed with aqueous sodium carbonate solution
  4. dry with materialdried with calcium chloride
  5. customThe solvent is evaporated
  6. customthe residue recrystallized several times from aqueous methanol

출처 및 근거

ORD 기록
ord-6a17fcba63804977894d0c2c861704a7
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04140843

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