4-Chlorophenyl Isocyanate → 1-(4-Chlorophenyl)-3-(1-methyl-2-piperidylidene)urea

HRID 2071524노트

반응식

HRID 2071524 반응식
[NH:1]=[C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[CH3:8].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]=[C:17]=[O:18])=[CH:12][CH:11]=1>C1C=CC=CC=1>[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]([N:1]=[C:2]2[CH2:7][CH2:6][CH2:5][CH2:4][N:3]2[CH3:8])=[O:18])=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 76934-Chlorophenyl IsocyanateHCID 124490281-Methylpiperidin-2-imine

생성물 1

HCID 536898361-(4-Chlorophenyl)-3-(1-methyl-2-piperidylidene)urea

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

The hydrochloride salt of 2-imino-1-methylpiperidine (7.43 g.; 0.05 mole) is converted to the free base in benzene in the usual manner. After drying over K2CO3 and filtering, a benzene solution of 0.05 mole of p-chlorophenylisocyanate is added dropwise with stirring. After addition is complete, further stirring is continued for about 6 hours at room temperature. The benzene is evaporated in vacuo and the solid residue is recrystallized from methanol to give the product, 1-(4-chlorophenyl)-3-(1-methyl-2-piperidylidene)urea.

후처리

  1. dry with materialAfter drying over K2CO3
  2. filtrationfiltering
  3. additionAfter addition
  4. stirringfurther stirring
  5. customThe benzene is evaporated in vacuo
  6. customthe solid residue is recrystallized from methanol

출처 및 근거

ORD 기록
ord-162246a195174ef8aee1f169e9820df3
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046909

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