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

HRID 1973952ノート

反応式

HRID 1973952 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 K 2 CO 3 and filtering, a benzene solution of 0.05 mole of p-chlorophenylisocvanate 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 K 2 CO 3
  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-7dcfc03d3b2641599763f0f53e3db97d
出典データセット
uspto-grants-1976_12
特許番号
US03998958

反応ノート

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