HRID518685
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To an ice-bath cooled suspension of cis-4-(2-chloro-5-nitropyridin-4-ylamino)-N-isopropylcyclohexanecarboxamide (400 mg, 1.174 mmol) in THF (2.3 mL) was added sodium methoxide (25 wt. % in MeOH (0.859 mL, 3.76 mmol)). The mixture was stirred in an ice bath for 1 minute. The ice bath was removed and the reaction was stirred for 30 minutes. The mixture was diluted with 10% IPA/DCM (5 mL) and washed with saturated aqueous NaHCO3 (1 mL). The layers were separated, and the organic layer was dried with Na2SO4 and the mixture purified via flash chromatography using a linear gradient of 0% to 5% of 1% NH4OH in MeOH in DCM. The title compound was collected as a yellow solid (289 mg, 73%).
WORKUP
后处理
- temperatureTo an ice-bath cooled
- customThe ice bath was removed
- stirringthe reaction was stirred for 30 minutes
- additionThe mixture was diluted with 10% IPA/DCM (5 mL)
- washwashed with saturated aqueous NaHCO3 (1 mL)
- customThe layers were separated
- dry with materialthe organic layer was dried with Na2SO4
- customthe mixture purified via flash chromatography
- customThe title compound was collected as a yellow solid (289 mg, 73%)