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

HRID 262764

반응식

HRID 262764 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[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1.C(O)C>O>[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[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)=[NH:11]

참가 물질

5

반응물 3

HCID 702EthanolHCID 310183-PyridinemethanamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

생성물 1

HCID 1785121111-(2,6-Dichlorobenzylideneamino)-3-(3-pyridylmethyl)guanidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5.85 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydriodide, 3.24 g. of 3-(aminomethyl)pyridine and 25 ml. of absolute ethanol is heated under reflux for 24 hours and diluted while hot with 75 ml. of water. After cooling, an oil separates and crystallizes. The mixture is chilled overnight and the crystals are separated and recrystallized from 100 ml. of 50% aqueous ethanol to give the desired product as pale yellow crystals, m.p. 148°-151° C.

후처리

  1. additionA mixture of 5.85 g
  2. temperatureunder reflux for 24 hours
  3. additiondiluted while hot with 75 ml
  4. temperatureAfter cooling
  5. customan oil separates and crystallizes
  6. temperatureThe mixture is chilled overnight
  7. customthe crystals are separated
  8. customrecrystallized from 100 ml

출처 및 근거

ORD 기록
ord-8c8de0a855b04af48e24d7a007cf8f02
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154947

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