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

HRID 37296

반응식

HRID 37296 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-03085be664434eebbe7e6fc4b41d7bde
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420164

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