반응 #576981

반응 방정식

1,1-dimethylethyl 4-[({[6-amino-5-chloro-2-(methyloxy)-3-pyridinyl]carbonyl}amino)methyl]-1-piperidinecarboxylate

→

title compound

수율 85.1%

6-Amino-5-chloro-2-(methyloxy)-N-(4-piperidinylmethyl)-3-pyridinecarboxamide

수율 85.1%

용매

hydrochloric acid

반응 조건

후처리

1. 1
   농축The mixture was concentrated to ca. 30 ml
2. 2
   추출the aqueous layer was extracted with dichloromethane (80 ml×3)
3. 3
   건조The combined organic layer was dried over magnesium sulfate
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:15)

실험 절차

A solution of 1,1-dimethylethyl 4-[({[6-amino-5-chloro-2-(methyloxy)-3-pyridinyl]carbonyl}amino)methyl]-1-piperidinecarboxylate (step 1 in example 1, 6.20 g, 15.5 mmol) in 10% methanolic hydrochloric acid (130 ml) was stirred at room temperature for 7 h. The mixture was concentrated to ca. 30 ml. The residue was basified with 2 N aqueous sodium hydroxide (pH=10) and the aqueous layer was extracted with dichloromethane (80 ml×3). The combined organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:15) to give 3.94 g (85%) of the title compound as a white solid.

출처