反応 #2321609

反応方程式

DIPEA

2-Aminothiazole-4-carboxylate hydrobromide salt

HATU

4-amino-1-methylpiperidine

→

title compound

収率 53.0%

2-amino-N-(1-methyl-4-piperidyl)-1,3-thiazole-4-carboxamide

収率 53.0%

溶媒

DMF

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated
2. 2
   その他absorbed onto an SCX column
3. 3
   洗浄washed with methanol
4. 4
   洗浄eluted with ammonia in methanol
5. 5
   workup.ADDITIONProduct containing fractions
6. 6
   その他evaporated
7. 7
   その他the residue and further purified by column chromatography (5% 7N NH3 in MeOH/DCM) Product
8. 8
   workup.ADDITIONcontaining fractions
9. 9
   その他evaporated

実験手順

2-Aminothiazole-4-carboxylate hydrobromide salt (Chempacific; 1.13 g, 5.02 mmol), HATU (2.87 g, 7.53 mmol) and 4-amino-1-methylpiperidine (0.86 g, 7.53 mmol) were stirred in DMF (5 mL) and DIPEA (5.2 mL, 30.12 mmol) added. The mixture was stirred at room temperature overnight. The reaction mixture was concentrated and the residue taken up in methanol, absorbed onto an SCX column, washed with methanol and eluted with ammonia in methanol. Product containing fractions were combined, evaporated and the residue and further purified by column chromatography (5% 7N NH3 in MeOH/DCM) Product containing fractions were combined and evaporated to give the title compound as a yellow solid (635 mg, 53%).

出典