Triethylamine → Methyl 4-{[1-(3,4-dichlorobenzyl)-4-piperidinyl]amino}-4-oxobutanoate

HRID 1070497노트

반응식

HRID 1070497 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][C:16]=1[Cl:17])[CH2:6][N:7]1[CH2:12][CH2:11][CH:10]([NH2:13])[CH2:9][CH2:8]1.Cl[C:19](=[O:26])[CH2:20][CH2:21][C:22]([O:24][CH3:25])=[O:23].C(N(CC)CC)C.C(=O)([O-])O.[Na+]>ClCCl>[Cl:2][C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][C:16]=1[Cl:17])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH:13][C:19](=[O:26])[CH2:20][CH2:21][C:22]([O:24][CH3:25])=[O:23])[CH2:11][CH2:12]1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 73888Butanoic acid, 4-chloro-4-oxo-, methyl esterHCID 516892Sodium BicarbonateHCID 223962061-(3,4-Dichloro-benzyl)-piperidin-4-ylamine hydrochloride

생성물 1

HCID 22396186Methyl 4-{[1-(3,4-dichlorobenzyl)-4-piperidinyl]amino}-4-oxobutanoate수율 67.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(3,4-dichlorobenzyl)-4-piperidinamine hydrochloride (3.50 g) in dichloromethane (100 ml) was added methyl 4-chloro-4-oxobutanoate (2.00 g) dropwise. Triethlamine (3.90 g) was added and the reaction stirred under nitrogen for 2 hours. Saturated sodium hydrogen carbonate solution was then added, with the solution being extracted three times with dichloromethane. The pooled organic phase was washed once with water, once with saturated brine and dried over anhydrous magnesium sulfate. After filtration the solvent was removed under reduced pressure to leave methyl 4-{[1-(3,4-dichlorobenzyl)-4-piperidinyl]amino}-4-oxobutanoate (3.00 g).

후처리

  1. extractionbeing extracted three times with dichloromethane
  2. washThe pooled organic phase was washed once with water, once with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtration the solvent
  5. customwas removed under reduced pressure

출처 및 근거

ORD 기록
ord-8d5f1eea97bc47f98bbd7a892febd140
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903085B1

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