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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 5-Phenyl-pyridine-2-carboxylic acid {2-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide

HRID 1177943
ノート
印刷プレビュー

反応式

HRID 1177943 の反応式
CCN(C(C)C)C(C)C.[C:10]1([C:16]2[CH:17]=[CH:18][C:19]([C:22]([NH:24][CH2:25][C:26]([OH:28])=O)=[O:23])=[N:20][CH:21]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[F:51][C:52]1[CH:53]=[CH:54][C:55]([C:66]([F:69])([F:68])[F:67])=[C:56]([C:58]([N:60]2[CH2:65][CH2:64][NH:63][CH2:62][CH2:61]2)=[O:59])[CH:57]=1>CN(C=O)C.O>[F:51][C:52]1[CH:53]=[CH:54][C:55]([C:66]([F:68])([F:67])[F:69])=[C:56]([CH:57]=1)[C:58]([N:60]1[CH2:61][CH2:62][N:63]([C:26](=[O:28])[CH2:25][NH:24][C:22]([C:19]2[CH:18]=[CH:17][C:16]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[CH:21][N:20]=2)=[O:23])[CH2:64][CH2:65]1)=[O:59]
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 57874442[(5-Phenyl-pyridine-2-carbonyl)-amino]-acetic acidHCID 66625607(2-Trifluoromethyl-5-fluoro-phenyl)-piperazin-1-yl-methanone hydrochloride

生成物 1

HCID 25165328
5-Phenyl-pyridine-2-carboxylic acid {2-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide
収率 39%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

DIPEA (151 mg, 0.2 mL, 1.17 mmol) was added to a stirred solution of [(5-phenyl-pyridine-2-carbonyl)-amino]-acetic acid (100 mg, 0.39 mmol) in DMF (2 mL). HOBT (63 mg, 0.46 mmol) and EDCI (89 mg, 0.46 mmol) were then added at room temperature. After 2 minutes, (5-fluoro-2-trifluoromethyl-phenyl)-piperazin-1-yl-methanone hydrochloride salt (146 mg, 0.46 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 afford 78 mg (39% yield) of 5-phenyl-pyridine-2-carboxylic acid {2-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide. LCMS Purity: 95.81%. 1H NMR (DMSO-d6): δ 9 (s, 1H), 8.8 (bt, 1H), 8.3 (d, 1H), 8.1 (m, 1H), 7.9 (m, 1H), 7.8 (d, 1H), 7.6-7.4 (m, 5H), 4.4-4.2 (dd, 2H), 3.8-3.4 (m, 6H), 3.3-3.1 (m, 2H).

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

出典と根拠

ORDレコード
ord-5b9f3f7dab2f4136ba8c2cacb9abc95a
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

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