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

HRID 64648ノート

反応式

HRID 64648 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ea7863179ebd4bd8baa5658f7a499e8f
出典データセット
uspto-grants-1986_09
特許番号
US04609669

反応ノート

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