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

HRID 1241898
ノート
印刷プレビュー

反応式

HRID 1241898 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9835a220bb114b1aaf88c848ab885bc4
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07115635B2

反応ノート

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