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

HRID 415264

反応式

HRID 415264 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH2:14][CH:13]([C:17](Cl)=[O:18])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[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>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH2:14][CH:13]([C:17](=[O:18])[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])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 (0.85 g, 3 mmol) and methyl 3-amino-2-hydroxybenzoate (0.6 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 of 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-faafd834cb3742299273fd569fedd672
出典データセット
uspto-grants-2012_01
特許番号
US08088760B2

関連ノート

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