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Hydrochloric Acid → S-[2-(5-methyl-4-imidazolylmethylthio)ethyl]-N-cyano-N'-methylisothiourea hydrochloride

HRID 46483
ノート
印刷プレビュー

反応式

HRID 46483 の反応式
[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][S:8][CH2:9][CH2:10][SH:11].[ClH:12].[C:13]([NH:15][C:16](=[N:19][CH3:20])SC)#[N:14]>N1C=CC=CC=1.O>[ClH:12].[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][S:8][CH2:9][CH2:10][S:11][C:16](=[N:19][CH3:20])[NH:15][C:13]#[N:14]
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 3

HCID 313Hydrochloric Acid2 回HCID 1111031-Cyano-2,3-dimethylisothioureaHCID 203874282-(5-Methyl-4-imidazolylmethylthio)ethanethiol

生成物 1

HCID 20387431S-[2-(5-methyl-4-imidazolylmethylthio)ethyl]-N-cyano-N'-methylisothiourea hydrochloride

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 1049
Pyridine
溶媒

実験手順

2-(5-Methyl-4-imidazolylmethylthio)ethanethiol (4.0 g) (prepared from the hydrochloride as in Example 1(b) and N-cyano-N', S-dimethylisothiourea (4.0 g) were heated together under nitrogen in pyridine (100 ml) at 100° for 20 hours. After this time the mixture was evaporated to dryness to give the crude title product. This residue taken up in water acidified to pH2 with concentrated hydrochloric acid. After extracting with ethyl acetate the volume of the aqueous fraction was reduced and on cooling gave S-[2-(5-methyl-4-imidazolylmethylthio)-ethyl]-N-cyano-N'-methylisothiourea hydrochloride, m.p. 225°.

後処理

  1. customAfter this time the mixture was evaporated to dryness
  2. customto give the crude title product
  3. extractionAfter extracting with ethyl acetate the volume of the aqueous fraction
  4. temperatureon cooling

出典と根拠

ORDレコード
ord-28bf5f7a742441e182c789e0a51bc023
出典データセット
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04173644

反応ノート

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