1-Butanol → 1-{[1-(p-Chlorophenyl)cyclopropyl]methyl}-3-(2,6-dichlorobenzylideneamino)guanidine

HRID 2419790

반응식

HRID 2419790 반응식
I.[Cl:2][C:3]1[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[C:4]=1[CH:5]=[N:6][NH:7][C:8](=[NH:11])SC.[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2([CH2:27][NH2:28])[CH2:26][CH2:25]2)=[CH:20][CH:19]=1.C(O)CCC>O.C(OCC)(=O)C>[Cl:17][C:18]1[CH:19]=[CH:20][C:21]([C:24]2([CH2:27][NH:28][C:8]([NH:7][N:6]=[CH:5][C:4]3[C:12]([Cl:16])=[CH:13][CH:14]=[CH:15][C:3]=3[Cl:2])=[NH:11])[CH2:25][CH2:26]2)=[CH:22][CH:23]=1

참가 물질

6

반응물 3

HCID 2631-ButanolHCID 4120166[1-(4-Chlorophenyl)cyclopropyl]methanamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

생성물 1

HCID 1785120881-{[1-(p-Chlorophenyl)cyclopropyl]methyl}-3-(2,6-dichlorobenzylideneamino)guanidine

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of 7.80 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide and 4.37 g. of 1-(p-chlorophenyl)cyclopropanemethylamine in 100 ml. of n-butanol and 25 ml. of water is heated at reflux for 24 hours. The solution is cooled, diluted with water to a final volume of 2 liters and allowed to stand. Filtration gives a tan solid which is dissolved in ethyl acetate and purified by silica gel column chromatography. Crystallization of the product from diethyl ether gives the desired final product as colorless crystals, m.p. 126°-128° C.

후처리

  1. temperatureat reflux for 24 hours
  2. temperatureThe solution is cooled
  3. filtrationFiltration
  4. customgives a tan solid which
  5. custompurified by silica gel column chromatography
  6. customCrystallization of the product from diethyl ether

출처 및 근거

ORD 기록
ord-4944ab98b94743809047afb25af45334
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107326

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