Water → 1-(1-Methyl-2-piperidylidene)-3-(4-trifluoromethylphenyl)urea

HRID 2071523노트

반응식

HRID 2071523 반응식
[NH:1]=[C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[CH3:8].[OH-].[Na+].O.[F:12][C:13]([F:24])([F:23])[C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:21]=[O:22])=[CH:16][CH:15]=1>CO>[CH3:8][N:3]1[CH2:4][CH2:5][CH2:6][CH2:7][C:2]1=[N:1][C:21]([NH:20][C:17]1[CH:16]=[CH:15][C:14]([C:13]([F:12])([F:23])[F:24])=[CH:19][CH:18]=1)=[O:22]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 737684-(Trifluoromethyl)phenyl isocyanateHCID 124490281-Methylpiperidin-2-imine

생성물 1

HCID 542292351-(1-Methyl-2-piperidylidene)-3-(4-trifluoromethylphenyl)urea

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The hydrochloride salt of 2-imino-1-methylpiperidine (7.60 g.; 0.068 mole) is converted to free base by adding 7 ml. of NaOH (50%) to an aqueous slurry (using a minimal amount of water) of the salt and then extracting with benzene. After drying over K2CO3, the benzene solution is filtered through diatomaceous earth. A benzene solution of 12.73 g. (0.068 mole) of p-trifluoromethylphenylisocyanate [prepared according to Inukai and Maki, Kogyo Kagaku Zasshi, 67 (5) 807-9 (1964] is added to the above solution slowly. After 4 hours of stirring at room temperature, the benzene is evaporated in vacuo to give a solid residue. Repeated recrystallizatons of the solid from methanol yields the pure product, 1-(1-methyl-2-piperidylidene)-3-(4-trifluoromethylphenyl)urea, m.p. = 154°-155° C.

후처리

  1. additionby adding 7 ml
  2. extractionextracting with benzene
  3. dry with materialAfter drying over K2CO3
  4. filtrationthe benzene solution is filtered through diatomaceous earth
  5. additionis added to the above solution slowly
  6. customthe benzene is evaporated in vacuo
  7. customto give a solid residue

출처 및 근거

ORD 기록
ord-cc533664f58a47ee956e181f1746cd86
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046909

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