Methyltriphenylphosphonium iodide → 1,2-Bis(difluoromethoxy)-4-vinylbenzene

HRID 1992347노트

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HRID 1992347 반응식
[CH3:1]C(C)([O-])C.[K+].[I-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[F:28][CH:29]([F:43])[O:30][C:31]1[CH:32]=[C:33]([CH:36]=[CH:37][C:38]=1[O:39][CH:40]([F:42])[F:41])[CH:34]=O>C1COCC1>[F:41][CH:40]([F:42])[O:39][C:38]1[CH:37]=[CH:36][C:33]([CH:34]=[CH2:1])=[CH:32][C:31]=1[O:30][CH:29]([F:43])[F:28]

참가 물질

5

반응물 3

HCID 638159Methyltriphenylphosphonium iodideHCID 145092693,4-Bis(difluoromethoxy)benzaldehydeHCID 23665647Potassium tert-butoxide

생성물 1

HCID 685199461,2-Bis(difluoromethoxy)-4-vinylbenzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Potassium tert-butoxide (6.7 g, 0.0683 mol) was taken in dry THF (25 mL) and stirred at 0° C. under a nitrogen atmosphere for 15 min. Methyl triphenylphosphonium iodide (27.6 g, 0.0683 mol; see step (ii) above) was then added, followed by 3,4-bis(difluoromethoxy)benzaldehyde (8 g, 0.034 mol; see step (i) above). The reaction mixture was then stirred for 1 h at RT, before being quenched with water. The organic solvents were evaporated under reduced pressure and the aqueous layer extracted with dichloromethane. Evaporation of the solvents followed, by chromatography of the residue over silica gel (using petroleum ether in ethyl acetate as eluent) afforded the sub-title compound as a pale yellow liquid. Yield: 6.5 g

후처리

  1. stirringThe reaction mixture was then stirred for 1 h at RT
  2. custombefore being quenched with water
  3. customThe organic solvents were evaporated under reduced pressure
  4. extractionthe aqueous layer extracted with dichloromethane
  5. customEvaporation of the solvents

출처 및 근거

ORD 기록
ord-5659e3aad312417791223a22e8bd8b96
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648985B2

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