Epichlorohydrin → 2-Ethoxy-1-methylpyridinium fluoroborate

HRID 67179

반응식

HRID 67179 반응식
C(C1OC1)Cl.B(F)(F)F.[CH3:10][CH2:11][O:12][CH2:13][CH3:14].[F:15][B-:16]([F:19])([F:18])[F:17].[CH2:20]([O+:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH3:21].[CH3:27][N:28]1C=C[CH:31]=[CH:30][C:29]1=O>CCOCC.C(Cl)Cl>[F:15][B-:16]([F:19])([F:18])[F:17].[CH2:20]([O+:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH3:21].[F:15][B-:16]([F:19])([F:18])[F:17].[CH2:11]([O:12][C:13]1[CH:14]=[CH:31][CH:30]=[CH:29][N+:28]=1[CH3:27])[CH3:10]

참가 물질

8

반응물 4

HCID 7835EpichlorohydrinHCID 8000Boron trifluoride etherateHCID 127551-Methyl-2(1H)-pyridinoneHCID 2723982Triethyloxonium tetrafluoroborate

생성물 2

HCID 2723982Triethyloxonium tetrafluoroborateHCID 130594562-Ethoxy-1-methylpyridinium fluoroborate수율 71%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 6344Dichloromethane용매2회

실험 절차

Triethyloxonium fluoroborate is prepared from 3.70 g (0.040 mole) of epichlorohydrin in 14 ml of ether and 7.58 g (0.054 mole) of boron trifluoride etherate in 6 ml of ether. The resulting solid triethyloxonium tetrafluoroborate is dissolved in 20 ml of dry methylene chloride and treated under nitrogen with 4.36 g (0.040 mole) of 1-methyl-2-pyridone in 15 ml of methylene chloride. The reaction mixture is stirred under nitrogen at room temperature overnight (about 16 hours). The solvent is evaporated at room temperature, in vacuo and the quaternary salt obtained is recrystallized from methanol-ether (1:1) to give 8.0 g (71%) of 2-ethoxy-1-methylpyridinium fluoroborate, m.p. 58°-60° C.

후처리

  1. customThe solvent is evaporated at room temperature, in vacuo
  2. customthe quaternary salt obtained
  3. customis recrystallized from methanol-ether (1:1)

출처 및 근거

ORD 기록
ord-184a5348c3a84a9f84afde24a9c1123e
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04345083

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