Potassium Carbonate → 2-Chloro-5-{[2-(nitromethylidene)imidazolidin-1-yl]methyl}pyridine

HRID 35737

반응식

HRID 35737 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH2:11][NH2:12])=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].F[C:20](F)(F)[CH2:21][N+:22]([O-:24])=[O:23]>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[CH2:10][CH2:11][NH:12][C:20]2=[CH:21][N+:22]([O-:24])=[O:23])=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5227621,1,1-Trifluoro-2-nitroethaneHCID 10997737N-[(6-Chloro-3-pyridinyl)methyl]-1,2-ethanediamine

생성물 1

HCID 1809572-Chloro-5-{[2-(nitromethylidene)imidazolidin-1-yl]methyl}pyridine수율 70.1%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
20 °C

실험 절차

5 g (26.9 mmol) of N-(2-chloro-5-pyridylmethyl)ethylene-diamine and 11.7 g (84.6 mmol) of potassium carbonate are placed in 40 ml of methanol. A solution of 3.64 g (28.2 mmol) of 1,1,1-trifluoro-2-nitro-ethane in 20 ml of methanol is added dropwise at 5° C. to 10° C. within 30 minutes. After the addition is complete, the mixture is stirred for 5 hours at 20° C. The mixture is then concentrated by removal of the solvent by distillation in vacuo, and the residue is taken up in methylene chloride, washed with a small amount of water, dried, concentrated and recrystallized from methanol. 4.6 g (70.1% of theory) of 1-(2-chloro-5-pyridylmethyl)-2-(nitromethylene)-imidazoline of a melting point of 160° C. to 161° C. are obtained.

후처리

  1. additionAfter the addition
  2. concentrationThe mixture is then concentrated by removal of the solvent by distillation in vacuo
  3. washwashed with a small amount of water
  4. customdried
  5. concentrationconcentrated
  6. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-49abe6dc727b45378bf0d7da4fc51e53
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767864

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