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

HRID 1112213
ノート
印刷プレビュー

反応式

HRID 1112213 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-4502fce072894240973d9dbc7c8b0ef5
出典データセット
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04120966

反応ノート

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