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Monomethylamine methanol → N-(2-chloro-5-thiazolylmethyl)-N'-methyl-N"-nitroguanidine

HRID 1275361
ノート
印刷プレビュー

反応式

HRID 1275361 の反応式
CO.[CH3:3][NH2:4].[Cl:5][C:6]1[S:7][C:8]([CH2:11][NH:12][C:13](=[N:16][N+:17]([O-:19])=[O:18])SC)=[CH:9][N:10]=1>C(#N)C>[Cl:5][C:6]1[S:7][C:8]([CH2:11][NH:12][C:13]([NH:4][CH3:3])=[N:16][N+:17]([O-:19])=[O:18])=[CH:9][N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 57454252Monomethylamine methanolHCID 136331499N-(2-chloro-5-thiazolylmethyl)-S-methyl-N'-nitroisothiourea

生成物 1

HCID 135779804N-(2-chloro-5-thiazolylmethyl)-N'-methyl-N"-nitroguanidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

349 mg of a 40% methylamine methanol solution was dropwise added to a mixture consisting of 1 g N-(2-chloro-5-thiazolylmethyl)-S-methyl-N'-nitroisothiourea and 30 ml acetonitrile, at room temperature, over 5 minutes. After stirring for 1.5 hours, the resultant white precipitate was collected by filtration and then dried to afford 410 mg of N-(2-chloro-5-thiazolylmethyl)-N'-methyl-N"-nitroguanidine (compound No.14) as a white powder. The mother liquor after the filtration was concentrated, then 20 ml of ethanol was added, followed by stirring thoroughly, and the crystals formed were collected by filtration to obtain additional 330 mg of compound No.14 (mp 172-173° C.). Upon recrystallization from acetonitrile, this product exhibited mp 173-174° C.

後処理

  1. filtrationthe resultant white precipitate was collected by filtration
  2. customdried

出典と根拠

ORDレコード
ord-b4e715ef19a14c548a36b1db66ec3d12
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06160126

反応ノート

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