Potassium Carbonate → Ethyl 1-((2-(4-chlorophenyl)-5-methyloxazol-4-yl)methyl)piperidine-4-carboxylate

HRID 1025403ノート

反応式

HRID 1025403 の反応式
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[O:6][C:7]=1[CH3:8].[NH:16]1[CH2:21][CH2:20][CH:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:18][CH2:17]1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([C:5]2[O:6][C:7]([CH3:8])=[C:3]([CH2:2][N:16]3[CH2:21][CH2:20][CH:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:18][CH2:17]3)[N:4]=2)=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70770Ethyl 4-piperidinecarboxylateHCID 36136584-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole

生成物 1

HCID 42116034Ethyl 1-((2-(4-chlorophenyl)-5-methyloxazol-4-yl)methyl)piperidine-4-carboxylate収率 91%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

The mixture of 4-(chloromethyl)-2-(4-chlorophenyl)-5-methyloxazole (1.21 g, 5 mmole, commercially from Fluorochem) and ethyl piperidine-4-carboxylate (0.81 mL, 1.05 equiv.), K2CO3 (1.03 g, 1.5 equiv) in dioxane was stirred at 70° C. for 2 h. The reaction solution was cooled to room temperature and the solid was filtered off, rinsed with dichloromethane. The filtrate was concentrated and the residue was recrystallized from hexane to furnish Ethyl 1-((2-(4-chlorophenyl)-5-methyloxazol-4-yl)methyl)piperidine-4-carboxylate (1.65 g, 91%).

後処理

  1. filtrationthe solid was filtered off
  2. washrinsed with dichloromethane
  3. concentrationThe filtrate was concentrated
  4. customthe residue was recrystallized from hexane

出典と根拠

ORDレコード
ord-82b9dc29de6a49b2897e37e278191044
出典データセット
uspto-grants-2014_05
特許番号
US08729081B2

反応ノート

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