反応 #96258

反応方程式

methanol

2-guanidino-4-[2-(2-cyano-3-methylguanidino)ethylthiomethyl]thiazole

hydrochloric acid

hydrogen chloride

→

2-guanidino-4-[2-(2-carbamoyl-3-methylguanidino)ethylthiomethyl]thiazole hydrochloride

反応条件

後処理

1. 1
   温度was heated for four minutes on the steam bath
2. 2
   温度On cooling a white solid
3. 3
   その他precipitated which
4. 4
   洗浄eluted with chloroform/methanol/ammonia (s.g. 0.880) 7:3:0.5 v/v/v
5. 5
   その他The yellow foam obtained
6. 6
   その他The solution was evaporated to dryness
7. 7
   その他the residue crystallized from methanol

実験手順

A mixture of 2-guanidino-4-[2-(2-cyano-3-methylguanidino)ethylthiomethyl]thiazole (1.0 g.), and 2.5 N hydrochloric acid (12 ml.) was heated for four minutes on the steam bath. On cooling a white solid precipitated which was applied to Merck 60 F-254 preparative thin layer chromatography plates and eluted with chloroform/methanol/ammonia (s.g. 0.880) 7:3:0.5 v/v/v. The yellow foam obtained was dissolved in methanol and methanolic hydrogen chloride added. The solution was evaporated to dryness and the residue crystallized from methanol to give 2-guanidino-4-[2-(2-carbamoyl-3-methylguanidino)ethylthiomethyl]thiazole hydrochloride, m.p. 148°-150° C.

出典