2,6-Lutidine → HCID 21472403, 화합물

HRID 2294964노트

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HRID 2294964 반응식
[S:1]([O:8]S(C(F)(F)F)(=O)=O)([C:4]([F:7])([F:6])[F:5])(=[O:3])=[O:2].[CH2:16]([C:19]1[CH:24]=[C:23]([N+:25]([O-:27])=[O:26])[CH:22]=[CH:21][C:20]=1O)[CH:17]=[CH2:18].CC1C=CC=C(C)N=1>ClCCl>[O:8]([C:20]1[CH:21]=[CH:22][C:23]([N+:25]([O-:27])=[O:26])=[CH:24][C:19]=1[CH2:16][CH:17]=[CH2:18])[S:1]([C:4]([F:7])([F:6])[F:5])(=[O:3])=[O:2]

참가 물질

5

반응물 3

HCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydrideHCID 2584392-allyl-4-nitrophenol

생성물 1

HCID 21472403HCID 21472403, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triflic anhydride (1.63 ml) was added dropwise to a mixture of 2-allyl-4-nitrophenol (1.79 g) and 2,6-dimethylpyridine (1.18 g) in dry dichloromethane (15 ml) at -20° C. under an atmosphere of argon. The reaction mixture was allowed to reach ambient temperature over 3 hours. The mixture was partitioned between water and dichloromethane. The organic phase was separated, washed with 1M aqueous sodium hydroxide solution, water, dried (MgSO4) and evaporated to give 2-allyl-4-nitrophenyl triflate (2.71 g) as an oil; microanalysis, found: C, 38.7; H, 2.6; N, 4.2%; C10H8F3NO5S requires: C, 38.6; H, 2.59; N, 4.5%; NMR: 3.7(2H,d), 5.19-5.35(2H,m), 5.97-6.17(1H,m), 7.84(1H,d), 8.36-8.55(2H,m); m/z 311(M).

후처리

  1. customThe mixture was partitioned between water and dichloromethane
  2. customThe organic phase was separated
  3. washwashed with 1M aqueous sodium hydroxide solution, water
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-ada0f62e4dd9423da364c34733a04024
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691349

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