2,3,4,5,6-Pentafluorobenzyl Alcohol → Pentafluorobenzyl fluoride

HRID 354710

反応式

HRID 354710 の反応式
[F:1][C:2]1[C:7]([CH2:8]O)=[C:6]([F:10])[C:5]([F:11])=[C:4]([F:12])[C:3]=1[F:13].ClC(F)C(N(CC)CC)(F)[F:17]>C(Cl)Cl>[F:1][C:2]1[C:7]([CH2:8][F:17])=[C:6]([F:10])[C:5]([F:11])=[C:4]([F:12])[C:3]=1[F:13]

参加物

4

反応物 2

HCID 99232,3,4,5,6-Pentafluorobenzyl AlcoholHCID 1361842-Chloro-N,N-diethyl-1,1,2-trifluoroethan-1-amine

生成物 1

HCID 12701527Pentafluorobenzyl fluoride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of pentafluorobenzyl alcohol (3.0 g) and dry methylene dichloride (50 ml) was cooled to a temperature of 0° C. in an ice-bath and 2-chloro-1-diethylamino-1,1,2-trifluoroethane (4.3 g) was slowly added to the cooled, stirred mixture over a period of ten minutes. After standing for a period of 18 hr at 0° C. the reaction mixture was poured into ice and the organic layer was separated and washed with IM aqueous sodium carbonate solution. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed by distillation and the product was distilled under reduced pressure to give pentafluorobenzyl fluoride, b.p. 51° C. at 30 mm Hg.

後処理

  1. additionthe reaction mixture was poured into ice
  2. customthe organic layer was separated
  3. washwashed with IM aqueous sodium carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was removed by distillation
  6. distillationthe product was distilled under reduced pressure

出典と根拠

ORDレコード
ord-933997dc546f4109b08b91bff02b2dcd
出典データセット
uspto-grants-1983_03
特許番号
US04376784

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