Water → 3,3-Difluoro-3-methoxy-2-trifluoromethylpropene

HRID 492275ノート

反応式

HRID 492275 の反応式
[CH2:1](N(CC)CC)C.[CH2:8]=[C:9]([C:14]([O:17]S(F)(=O)=O)([F:16])[F:15])[C:10]([F:13])([F:12])[F:11].O>CO>[F:15][C:14]([F:16])([O:17][CH3:1])[C:9]([C:10]([F:13])([F:12])[F:11])=[CH2:8]

参加物

5

反応物 3

HCID 962WaterHCID 8471TriethylamineHCID 87741755CH2=C(CF3)CF2Oso2F

生成物 1

HCID 865909533,3-Difluoro-3-methoxy-2-trifluoromethylpropene収率 51.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Triethylamine (2.5 g, 0.02 mole) is added gradually to CH2═C(CF3)CF2OSO2F (5 g, 0.02 mole) in dry methanol (10 ml) at 10° C. After 20 minutes the reaction mixture is poured into water. The organic layer is separated, washed in turn in dilute aqueous HCl, water, sodium bicarbonate solution, and water, and then dried over MgSO4. Distillation of the dried mixture gives 3,3-difluoro-3-methoxy-2-trifluoromethylpropene (1.8 g, 50% yield). The isomer 1,1-difluoro-2-trifluoromethyl-3-methoxypropene (about 1%) and CH2═C(CF3)COOCH3 (about 3%) are also detected by gas chromatography-mass spectrometry (GC-MS).

後処理

  1. customThe organic layer is separated
  2. washwashed in turn in dilute aqueous HCl
  3. dry with materialwater, sodium bicarbonate solution, and water, and then dried over MgSO4
  4. distillationDistillation of the dried mixture

出典と根拠

ORDレコード
ord-512dccee168a482bac759cd65077d648
出典データセット
uspto-grants-2009_05
特許番号
US07531689B2

反応ノート

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