4-tert-Butylcatechol → 1-Ethenyl-4-(trifluoromethyl)benzene

HRID 1599719

反応式

HRID 1599719 の反応式
O[CH:2]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1)[CH3:3].S([O-])(O)(=O)=O.[K+].C(C1C=C(O)C(=CC=1)O)(C)(C)C>>[F:11][C:10]([F:12])([F:13])[C:7]1[CH:8]=[CH:9][C:4]([CH:2]=[CH2:3])=[CH:5][CH:6]=1

参加物

4

反応物 3

HCID 73814-tert-ButylcatecholHCID 1371861-[4-(Trifluoromethyl)phenyl]ethan-1-olHCID 516920Potassium bisulfate

生成物 1

HCID 27827981-Ethenyl-4-(trifluoromethyl)benzene

実験手順

To the compound (I) (27.0 g/0.142 mol) were added potassium hydrogensulfate (7 g) and 4-tert-butylcatechol (polymerization inhibitor, 0.01 g). The mixture was distilled at 150° to 180° C. using an oil bath to collect the whole distillate. Ether (20 ml) was added to the distillate, an ethereal layer was separated from water, and sodium sulfate was added to the layer for dehydration, followed by filtration. The ether was removed from the filtrate, to which 4-tert-butylcatechol was added again. The filtrate was then distilled at a reduced pressure, giving 4-trifluoromethylstyrene [compound (II)] represented by the formula CF3C6H4CH=CH2, b.p. 78°~80° C. (2660 Pa), colorless transparent liquid, yield 76.5%.

後処理

  1. distillationThe mixture was distilled at 150° to 180° C.
  2. distillationto collect the whole distillate
  3. additionEther (20 ml) was added to the distillate
  4. customan ethereal layer was separated from water, and sodium sulfate
  5. additionwas added to the layer for dehydration
  6. filtrationfollowed by filtration
  7. customThe ether was removed from the filtrate, to which 4-tert-butylcatechol
  8. additionwas added again
  9. distillationThe filtrate was then distilled at a reduced pressure

出典と根拠

ORDレコード
ord-43f30c9bfd4c414fa03ba9e02fc97d70
出典データセット
uspto-grants-1998_04
特許番号
US05741922

関連ノート

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