2-Chloroethanol → 2,2-Bis(trifluoromethyl)-1,3-dioxolane

HRID 1509794ノート

反応式

HRID 1509794 の反応式
[CH2:1](Cl)[CH2:2][OH:3].[F:5][C:6]([F:14])([F:13])[C:7]([C:9]([F:12])([F:11])[F:10])=[O:8].COC(C)(C)C.C(=O)([O-])[O-].[K+].[K+]>O>[F:5][C:6]([F:14])([F:13])[C:7]1([C:9]([F:12])([F:11])[F:10])[O:3][CH2:2][CH2:1][O:8]1

参加物

6

反応物 4

HCID 342-ChloroethanolHCID 11430Potassium CarbonateHCID 12695HexafluoroacetoneHCID 15413tert-Butyl methyl ether

生成物 1

HCID 1205602,2-Bis(trifluoromethyl)-1,3-dioxolane収率 62.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a 300 mL three-necked flask equipped with a gas-inlet tube, a reflux condenser, and a thermometer was charged 10.0 g (0.12 mol) of ethylene chlorohydrin beforehand, followed by cooling with ice. Then, 20.0 g (0.12 mol) of hexafluoroacetone was added through the gas-inlet tube. After completion of the addition, the whole was stirred for 15 minutes as it was and then 100 mL of t-butyl methyl ether was added. Then, 16.6 g (0.12 mol) of potassium carbonate was added portionwise over a period of 1 hour and, after completion of the addition, the whole was stirred as it was. The resulting mixture was poured into 100 mL of water and an organic layer was separated by two-layer separation in a separating funnel. The resulting organic layer was subjected to distillation under normal pressure to collect a fraction of 106° C. to 107° C. to obtain 15.8 g (purity 99%, yield 62.0%) of 2,2-bis(trifluoromethyl)-1,3-dioxolane (fluorinated acetal (E)).

後処理

  1. customInto a 300 mL three-necked flask equipped with a gas-inlet tube, a reflux condenser
  2. temperatureby cooling with ice
  3. additionAfter completion of the addition
  4. additionafter completion of the addition
  5. stirringthe whole was stirred as it
  6. customan organic layer was separated by two-layer separation in a separating funnel
  7. distillationThe resulting organic layer was subjected to distillation under normal pressure
  8. customto collect a fraction of 106° C. to 107° C.

出典と根拠

ORDレコード
ord-9236dd49094a47558b6abc9de8560b02
出典データセット
uspto-grants-2012_07
特許番号
US08211612B2

反応ノート

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