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Triethylamine → 5-(4-acetylphenyl)-N-[1-(3,4-dichlorobenzyl)piperidin-4-yl]valeramide

HRID 1241898
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HRID 1241898 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][CH2:13][C:14]([OH:16])=O)=[CH:6][CH:5]=1)(=[O:3])[CH3:2].Cl.Cl.[NH2:19][CH:20]1[CH2:25][CH2:24][N:23]([CH2:26][C:27]2[CH:32]=[CH:31][C:30]([Cl:33])=[C:29]([Cl:34])[CH:28]=2)[CH2:22][CH2:21]1.C(N(CC)CC)C.CCN=C=NCCCN(C)C.Cl>ClCCl>[C:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:10][CH2:11][CH2:12][CH2:13][C:14]([NH:19][CH:20]2[CH2:25][CH2:24][N:23]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([Cl:33])=[C:29]([Cl:34])[CH:28]=3)[CH2:22][CH2:21]2)=[O:16])=[CH:8][CH:9]=1)(=[O:3])[CH3:2]
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 219371095-(4-Acetylphenyl)valeric acidHCID 219371291-(3,4-Dichlorobenzyl)piperidin-4-ylamine dihydrochloride

생성물 1

HCID 102265315-(4-acetylphenyl)-N-[1-(3,4-dichlorobenzyl)piperidin-4-yl]valeramide수율 55.7%

시약·촉매·용매

1
HCID 6344Dichloromethane용매

실험 절차

5-(4-Acetylphenyl)valeric acid (996 mg) and 4-amino-1-(3,4-dichlorobenzyl)piperidine dihydrochloride (1.50 g) were suspended in dichloromethane (40 mL), and triethylamine (1.26 mL) and EDC hydrochloride (953 mg) were added to the suspension. The suspension was stirred for 12 hrs. The reaction mixture was washed with water and then saturated brine and dried, and the solvent was evaporated under reduced pressure. Diethyl ether was added to the residue to crystallize to give the title compound (1.16 g) as a white solid.

후처리

  1. washThe reaction mixture was washed with water
  2. dry with materialsaturated brine and dried
  3. customthe solvent was evaporated under reduced pressure
  4. additionDiethyl ether was added to the residue
  5. customto crystallize

출처 및 근거

ORD 기록
ord-9835a220bb114b1aaf88c848ab885bc4
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07115635B2

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