Hydrochloric Acid → N-(Cyclohexylmethyl)-N'-(2,6-diethylphenyl)-N-(4-phenylcyclohexyl)carbamimidic acid

HRID 37296

反応式

HRID 37296 の反応式
[C:1]1([CH:7]2[CH2:12][CH2:11][CH:10]([NH:13][CH2:14][CH:15]3[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]3)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.[CH2:27]([C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH2:35][CH3:36])[C:30]=1[N:37]=[C:38]=[O:39])[CH3:28].Cl>ClCCl>[CH2:27]([C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH2:35][CH3:36])[C:30]=1[NH:37][C:38]([N:13]([CH2:14][CH:15]1[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]1)[CH:10]1[CH2:9][CH2:8][CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:12][CH2:11]1)=[O:39])[CH3:28]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 51531832,6-Diethylphenyl isocyanateHCID 19935094N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine

生成物 1

HCID 3072997N-(Cyclohexylmethyl)-N'-(2,6-diethylphenyl)-N-(4-phenylcyclohexyl)carbamimidic acid収率 36.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the solution of 2 g of N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine in dichloromethane was added 2 ml of pyridine and to the mixture was added a solution of 1.6 g of 2,6-diethylphenylisocyanate in 30 ml of dichloromethane dropwise. After the mixture was stirred at room temperature, to the solution was added diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, aqueous sodium hydrogencarbonate solution and saturated brine and then dried over magnesium sulfate. The solvent was distilled away in vacuo to give 2 g of crude crystals. The crystals were recrystallized from the mixture of ethyl acetate and hexane to give 1.2 g of N-(2,6-diethylphenyl)-N'-cyclohexylmethyl-N'-(4-phenylcyclohexyl)urea, melting at 166°-168° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water, aqueous sodium hydrogencarbonate solution and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled away in vacuo
  5. customto give 2 g of crude crystals
  6. customThe crystals were recrystallized from the mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-03085be664434eebbe7e6fc4b41d7bde
出典データセット
uspto-grants-1995_05
特許番号
US05420164

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