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

HRID 894347

反応式

HRID 894347 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. additionat 0° C. the 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-2dee3815e22a40a29f55ff6192862c75
出典データセット
uspto-grants-1981_08
特許番号
US04283414

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