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

HRID 262764

反応式

HRID 262764 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: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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c8de0a855b04af48e24d7a007cf8f02
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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