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Potassium Carbonate → 1-(Tert-butoxycarbonyl)piperidine-3,5-dicarboxylic acid

HRID 1698361
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HRID 1698361 반응식
C[O:2][C:3]([CH:5]1[CH2:10][CH:9]([C:11]([O:13]C)=[O:12])[CH2:8][N:7]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:6]1)=[O:4].C([O-])([O-])=O.[K+].[K+]>CO.O>[C:18]([O:17][C:15]([N:7]1[CH2:6][CH:5]([C:3]([OH:4])=[O:2])[CH2:10][CH:9]([C:11]([OH:13])=[O:12])[CH2:8]1)=[O:16])([CH3:21])([CH3:19])[CH3:20]
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 497610141-Tert-butyl 3,5-dimethyl piperidine-1,3,5-tricarboxylate

생성물 1

HCID 232911311-(Tert-butoxycarbonyl)piperidine-3,5-dicarboxylic acid

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

To a solution of piperidine-1,3,5-tricarboxylic acid 1-tert-butyl ester 3,5-dimethyl ester (6.8 g, 22.5 mmol) in MeOH/water (4:1, 120 mL), K2CO3 (9.4 g, 68 mmol) is added. The reaction is stirred at reflux overnight. The MeOH is evaporated and the residue extracted with dichloromethane and 1N aq. HCl. The organic phase is dried over Na2SO4, filtered and evaporated to give a light yellow solid. MS (LC-MS): 274 [M+H]+.

후처리

  1. temperatureat reflux overnight
  2. customThe MeOH is evaporated
  3. extractionthe residue extracted with dichloromethane and 1N aq. HCl
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give a light yellow solid

출처 및 근거

ORD 기록
ord-2255da03c43148c9adc17c1c80cf8fe6
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163773B2

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