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

HRID 2071524ノート

反応式

HRID 2071524 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-162246a195174ef8aee1f169e9820df3
出典データセット
uspto-grants-1977_09
特許番号
US04046909

反応ノート

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