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Hydrochloric Acid → HCID 178483280、化合物

HRID 482658
ノート
印刷プレビュー

反応式

HRID 482658 の反応式
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12][CH2:13][CH2:14][C:15]#[N:16])[CH:6]=1)[CH3:3].C(Cl)(Cl)Cl.Cl.[S:22]([NH2:26])([NH2:25])(=[O:24])=[O:23]>CO>[S:22]([NH:26][C:15](=[NH:16])[CH2:14][CH2:13][S:12][CH2:11][C:7]1[CH:6]=[C:5]([CH2:4][N:2]([CH3:3])[CH3:1])[CH:10]=[CH:9][N:8]=1)(=[O:24])(=[O:23])[NH2:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 82267SulfamideHCID 198704133-[({4-[(Dimethylamino)methyl]pyridin-2-yl}methyl)sulfanyl]propanenitrile

生成物 1

HCID 178483280HCID 178483280、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

3-(4-Dimethylaminomethyl-2-pyridylmethylthio)propionitrile in a mixture of dry methanol and dry chloroform under nitrogen at 2° C. is treated with dried hydrogen chloride gas and allowed to stand at ca. 0° C. to give after basification with ice cold potassium carbonate solution methyl-3-(4-dimethylaminomethyl-2-pyridylmethylthio)propionimidate which is reacted in methanol with sulphamide under reflux. Evaporation of the solvent at reduced pressure and purification of the product by chromatography yields N-sulphamoyl-3-(4-dimethylaminomethyl-2-pyridylmethylthio)propionamidine.

後処理

  1. customto stand at ca. 0° C.
  2. customto give after basification with ice cold potassium carbonate solution methyl-3-(4-dimethylaminomethyl-2-pyridylmethylthio)propionimidate which
  3. temperatureunder reflux
  4. customEvaporation of the solvent
  5. customat reduced pressure and purification of the product by chromatography

出典と根拠

ORDレコード
ord-95071697d3b04f27bdd22ffee558ca57
出典データセット
uspto-grants-1986_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04574126

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート