Methanol → Methyl 4-(piperidin-2-yl)butanoate hydrochloride

反応式

Cl.[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12].S(Cl)([Cl:16])=O.[CH3:18]O>>[ClH:16].[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([O:13][CH3:18])=[O:12]

参加物

反応物 3

HCID 887Methanol

HCID 24386Thionyl Chloride

HCID 124163274-(Piperidin-2-yl)butanoic acid--hydrogen chloride (1/1)

生成物 1

HCID 66772062Methyl 4-(piperidin-2-yl)butanoate hydrochloride収率 45%

実験手順

A solution of 4-(2-piperidinyl)butanoic acid hydrochloride (5.95 g, 34.8 mmol) in Methanol (104 ml) is cooled to 0° C. At this temperature thionylchloride (7.54 ml, 104.3 mmol) is added slowly. The reaction mixture is heated to reflux for 12 h. The solvent is evaporated in vacuum. The residue is suspended in Ethylacetate and is heated to reflux. The suspension is filtered while it is still hot. In the filtrate a white solid dropped out, which was filtered out and dried in vacuum to give Methyl 4-(piperidin-2-yl)butanoate hydrochloride (2) (3.49 g, 45%)