Ethanol → 1-(2,6-Dichlorobenzylideneamino)-3-(2-thenyl)guanidine

HRID 262768

반응식

HRID 262768 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.[NH2:17][CH2:18][C:19]1[S:20][CH:21]=[CH:22][CH:23]=1.C(O)C>O.[OH-].[Na+]>[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:17][CH2:18][C:19]1[S:20][CH:21]=[CH:22][CH:23]=1)=[NH:11]

참가 물질

6

반응물 3

HCID 702EthanolHCID 34005(2-Thienylmethyl)amineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

생성물 1

HCID 1785121161-(2,6-Dichlorobenzylideneamino)-3-(2-thenyl)guanidine

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of 5.85 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydriodide and 3.39 g. of 2-(aminomethyl)thiophene in 25 ml. of absolute ethanol is heated under reflux for 16 hours, diluted with water and excess 10N sodium hydroxide is added. After standing, crystallization occurs, and filtration gives 3.50 g. of nearly colorless crystals. Recrystallization from aqueous ethanol gives the desired product as colorless crystals, m.p. 135°-137° C.

후처리

  1. temperatureunder reflux for 16 hours
  2. additionis added
  3. customcrystallization
  4. filtrationfiltration
  5. customgives 3.50 g
  6. customRecrystallization from aqueous ethanol

출처 및 근거

ORD 기록
ord-99cc69d1626a41b6ac9ae6c77d9a89d0
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154947

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