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

HRID 262763노트

반응식

HRID 262763 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:24]=[CH:23][CH:22]=[CH:21][N:20]=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:24]=[CH:23][CH:22]=[CH:21][N:20]=1)=[NH:11]

참가 물질

5

반응물 3

HCID 702EthanolHCID 195092-PyridinemethanamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

생성물 1

HCID 1785121061-(2,6-Dichlorobenzylideneamino)-3-(2-pyridylmethyl)guanidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 5.85 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydriodide (U.S. Pat. No. 3,657,337) and 3.24 g. of 2-(aminomethyl)pyridine in 25 ml. of absolute ethanol is heated under reflux for 20 hours and diluted while hot with 75 ml. of water, causing the separation of an oil. On standing, the oil crystallizes and filtration gives 5.00 g. of pale yellow crystals, m.p. 125°-140° C. Recrystallization from aqueous ethanol gives the desired compound as pale yellow crystals, m.p. 159.5°-161° C.

후처리

  1. temperatureunder reflux for 20 hours
  2. additiondiluted while hot with 75 ml
  3. customthe separation of an oil
  4. customthe oil crystallizes
  5. filtrationfiltration
  6. customgives 5.00 g
  7. customRecrystallization from aqueous ethanol

출처 및 근거

ORD 기록
ord-e355e821ec8245679c76df6f123e72ba
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154947

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