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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-{2-Oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-4-piperidin-1-yl-benzamide

HRID 1177913
ノート
印刷プレビュー

反応式

HRID 1177913 の反応式
CCN(C(C)C)C(C)C.Cl.[NH2:11][CH2:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21](=[O:32])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[C:28]([F:31])([F:30])[F:29])[CH2:17][CH2:16]1)=[O:14].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[N:54]1([C:60]2[CH:68]=[CH:67][C:63]([C:64](O)=[O:65])=[CH:62][CH:61]=2)[CH2:59][CH2:58][CH2:57][CH2:56][CH2:55]1>CN(C=O)C.O>[O:14]=[C:13]([N:15]1[CH2:16][CH2:17][N:18]([C:21](=[O:32])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[C:28]([F:31])([F:29])[F:30])[CH2:19][CH2:20]1)[CH2:12][NH:11][C:64](=[O:65])[C:63]1[CH:67]=[CH:68][C:60]([N:54]2[CH2:59][CH2:58][CH2:57][CH2:56][CH2:55]2)=[CH:61][CH:62]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 7645994-(Piperidin-1-yl)benzoic acidHCID 669531782-Amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone hydrochloride

生成物 1

HCID 25166504
N-{2-Oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-4-piperidin-1-yl-benzamide
収率 21.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

DIPEA (188.6 mg, 0.25 mL, 1.45 mmol) was added to a stirred solution of 2-amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone hydrochloride salt (282.2 mg, 0.8 mmol) in DMF (4 mL). HOBT (108 mg, 0.8 mmol) and EDCI (279.7 mg, 1.45 mmol) were then added at room temperature. After 2 minutes, 4-piperidin-1-yl-benzoic acid (150 mg, 0.729 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and the product was extracted with EtOAc and the organic layer was washed with brine. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to get the residue. The obtained residue was purified by column chromatography (using silica gel of 60-120 mesh and 50% EtOAc in Hexane as eluent) to afford 80 mg (21.7% yield) N-{2-Oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-4-piperidin-1-yl-benzamide. LCMS Purity: 94.74%. 1H NMR (DMSO-d6): δ 8.2 (s, 1H), 7.9-7.5 (m, 6H), 7.0-6.9 (d, 2H), 4.2-4.0 (d, 2H), 3.8-3.5 (m, 4H), 3.35-3.2 (m, 4H), 3.2-3.0 (m, 4H), 1.7-1.5 (s, 6H).

後処理

  1. extractionthe product was extracted with EtOAc
  2. washthe organic layer was washed with brine
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customto get the residue
  6. customThe obtained residue was purified by column chromatography (using silica gel of 60-120 mesh and 50% EtOAc in Hexane as eluent)

出典と根拠

ORDレコード
ord-2ac5592878af4548bce4d2c452c17045
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842696B2

反応ノート

読み込み中…

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