benzyl 3-(chlorocarbonyl)tetrahydro-1(2H)-pyridinecarboxylate → Benzyl-3-(2-hydroxy-3-(methoxycarbonyl)phenylcarbamoyl)piperidine-1-carboxylate

HRID 415306

反応式

HRID 415306 の反応式
Cl[C:2]([CH:4]1[CH2:9][CH2:8][CH2:7][N:6]([C:10]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:11])[CH2:5]1)=[O:3].[NH2:20][C:21]1[C:22]([OH:31])=[C:23]([CH:28]=[CH:29][CH:30]=1)[C:24]([O:26][CH3:27])=[O:25]>ClCCl>[CH2:13]([O:12][C:10]([N:6]1[CH2:7][CH2:8][CH2:9][CH:4]([C:2](=[O:3])[NH:20][C:21]2[CH:30]=[CH:29][CH:28]=[C:23]([C:24]([O:26][CH3:27])=[O:25])[C:22]=2[OH:31])[CH2:5]1)=[O:11])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 2776575benzyl 3-(chlorocarbonyl)tetrahydro-1(2H)-pyridinecarboxylateHCID 12782444Methyl 3-amino-2-hydroxybenzoate

生成物 1

HCID 66621331Benzyl-3-(2-hydroxy-3-(methoxycarbonyl)phenylcarbamoyl)piperidine-1-carboxylate収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Benzyl 3-(chlorocarbonyl)piperidine-1-carboxylate (500 mg, 3 mmol) and methyl 3-amino-2-hydroxybenzoate (1.014 g, 3.6 mmol) were added in anhydrous dichloromethane (20 mL) and the mixture was stirred at room temperature overnight. The mixture was extracted with dichloromethane (100 mL×4) and the organic phase was dried with anhydrous sodium sulfate and evaporated under reduced pressure. 1.2 g benzyl-3-(2-hydroxy-3-(methoxycarbonyl)phenylcarbamoyl)piperidine-1-carboxylate was obtained. Yield: 97%. LC-MS (ESI) m/z: 413 (M+1)+.

後処理

  1. extractionThe mixture was extracted with dichloromethane (100 mL×4)
  2. dry with materialthe organic phase was dried with anhydrous sodium sulfate
  3. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-3803e9b9c49f4cbc82b19b5be917c2cc
出典データセット
uspto-grants-2012_01
特許番号
US08088760B2

関連ノート

読み込み中…