1-Methylimidazole → N-methyl-N-ethylimidazolium ethylethanephosphonate

HRID 1869618

반응식

HRID 1869618 반응식
[CH2:1]([O:3][P:4]([CH2:9][CH3:10])(=[O:8])[O:5]CC)[CH3:2].[CH3:11][N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1>>[CH2:1]([O:3][P:4]([CH2:9][CH3:10])(=[O:5])[O-:8])[CH3:2].[CH3:11][N+:12]1([CH2:9][CH3:10])[CH:16]=[CH:15][N:14]=[CH:13]1

참가 물질

3

반응물 2

HCID 13901-MethylimidazoleHCID 6534Diethyl ethylphosphonate

생성물 1

HCID 86609277N-methyl-N-ethylimidazolium ethylethanephosphonate수율 183.3%

실험 절차

Diethylethanephosphonate (68.2 g, 99%, 0.406 mole) was dripped into a 300 ml flask containing 33.3 g (99%, 0.402 mole) N-methylimidazole at 160° C. under nitrogen and stirring over a period of 80 minutes. The liquid was stirred at the same temperature for an additional 10 hours. The liquid was cooled, moved to a rotary evaporator and dried at 140° C./5 mmHg for 2.5 hours. The product (92.4 g, yield 92%) was a liquid at room temperature. 1H-NMR (CDCl3, 300.13 MHz, δ): 10.99 (s, 1H, —N—CH═N—), 7.73 (s, 1H, —N—CH═CH—N—), 7.65 (s, 1H, —N—CH═CH—N—), 4.39 (q, 2H, —N—CH2—CH3), 4.09 (s, 3H, —NCH3), 3.92 (m, 2H, —O—CH2—CH3), 1.56 (m, 3H, —OCH2—CH3), 1.56 (m, 2H, —(O═)P—CH2—CH3), 1.19 (m, 3H, —(O═)PCH2—CH3), 1.19 (m, 3H, —NCH2—CH3). 31P-NMR (CDCl3, 81.015 MHz, δ): 25.57 [s, RO—(R)P(═O)—O−].

후처리

  1. stirringThe liquid was stirred at the same temperature for an additional 10 hours
  2. temperatureThe liquid was cooled
  3. custommoved to a rotary evaporator
  4. customdried at 140° C./5 mmHg for 2.5 hours

출처 및 근거

ORD 기록
ord-d15ee3486d2945cf86386cc3a282cdad
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638636B2

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