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

HRID 262763

反応式

HRID 262763 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e355e821ec8245679c76df6f123e72ba
出典データセット
uspto-grants-1979_05
特許番号
US04154947

関連ノート

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