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

HRID 492275

반응식

HRID 492275 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 865909533,3-Difluoro-3-methoxy-2-trifluoromethylpropene수율 51.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-512dccee168a482bac759cd65077d648
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531689B2

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