1,2-Dibromoethane → 2-[2,6-Dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl bromide

HRID 256088노트

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HRID 256088 반응식
[Na].[Cl:2][C:3]1[CH:8]=[C:7]([S:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH:6]=[C:5]([Cl:15])[C:4]=1[OH:16].[CH2:17](Br)[CH2:18][Br:19]>C(O)C>[Cl:15][C:5]1[CH:6]=[C:7]([S:9][CH2:10][C:11]([F:13])([F:14])[F:12])[CH:8]=[C:3]([Cl:2])[C:4]=1[O:16][CH2:17][CH2:18][Br:19]

참가 물질

5

반응물 3

HCID 78391,2-DibromoethaneHCID 5360545SodiumHCID 136721742,6-Dichloro-4-(2,2,2-trifluoroethylthio)-phenol

생성물 1

HCID 136721752-[2,6-Dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl bromide수율 58.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

To an ethanol solution of sodium ethylate obtained by dissolving 0.7 g of metallic sodium in 50 ml of ethanol were added 8.9 g of 2,6-dichloro-4-(2,2,2,-trifluoroethylthio)-phenol and 20 g of ethylene bromide. The mixture was stirred at 40° C. for 2 hours and under reflux for 4 hours. Ethanol and the excess of ethylene bromide were evaporated. The residue was taken into 150 ml of toluene, washed with a 5% aqueous solution of potassium hydroxide and water in this sequence, and dried over anhydrous sodium sulfate. Toluene was evaporated, and the residue was distilled under reduced pressure to give 7.2 g of 2-[2,6-dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl bromide with the b.p.=124°-126° C./0.8 mmHg.

후처리

  1. temperatureunder reflux for 4 hours
  2. customEthanol and the excess of ethylene bromide were evaporated
  3. washwashed with a 5% aqueous solution of potassium hydroxide and water in this sequence
  4. dry with materialdried over anhydrous sodium sulfate
  5. customToluene was evaporated
  6. distillationthe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-dc0e2095a6584d94baa43709c4c22479
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04700006

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