Acetic Anhydride → 4-(6-(Acetamidomethyl)pyridin-2-yl)-2-guanidinothiazole

HRID 1491841ノート

反応式

HRID 1491841 の反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][CH2:9][C:10]1[N:15]=[C:14]([C:16]2[N:17]=[C:18]([N:21]=[C:22]([NH2:24])[NH2:23])[S:19][CH:20]=2)[CH:13]=[CH:12][CH:11]=1.C(=O)([O-])[O-].[K+].[K+]>N1C=CC=CC=1>[C:5]([NH:8][CH2:9][C:10]1[N:15]=[C:14]([C:16]2[N:17]=[C:18]([N:21]=[C:22]([NH2:24])[NH2:23])[S:19][CH:20]=2)[CH:13]=[CH:12][CH:11]=1)(=[O:7])[CH3:6]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 103997684-(6-Aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole

生成物 1

HCID 104469404-(6-(Acetamidomethyl)pyridin-2-yl)-2-guanidinothiazole

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Acetic anhydride was added dropwise to a solution of 4-(6-aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole (0.44 g) in pyridine (4.4 ml). After being stirred for two hours at ambient temperature, the mixture was mixed with aqueous potassium carbonate and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and evaporated in vacuo to give 4-(6-acetylaminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole. The residue was converted to the hydrochloride in a usual manner and the salt was recrystallized from a mixture of methanol and diisopropyl ether to give 4-(6-acetylaminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride (0.43 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-f9c3e787bb824cb1aab2bf913dce7a17
出典データセット
uspto-grants-1994_12
特許番号
US05371097

反応ノート

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