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1-Hydroxybenzotriazole → HCID 44231444、化合物

HRID 1665646
ノート
印刷プレビュー

反応式

HRID 1665646 の反応式
C1C=CC2N(O)N=NC=2C=1.[O:11]=[C:12]([N:17]1[CH2:22][CH2:21][N:20]([C:23](=[O:33])[C:24]2[CH:29]=[C:28]([F:30])[C:27]([F:31])=[C:26]([F:32])[CH:25]=2)[CH2:19][CH2:18]1)[CH2:13][C:14](O)=[O:15].CCN=C=NCCCN(C)C.Cl.[C:46]1([C:52]2[N:57]=[CH:56][C:55]([NH2:58])=[CH:54][CH:53]=2)[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[O:11]=[C:12]([N:17]1[CH2:22][CH2:21][N:20]([C:23](=[O:33])[C:24]2[CH:25]=[C:26]([F:32])[C:27]([F:31])=[C:28]([F:30])[CH:29]=2)[CH2:19][CH2:18]1)[CH2:13][C:14]([NH:58][C:55]1[CH:56]=[N:57][C:52]([C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)=[CH:53][CH:54]=1)=[O:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27628776-Phenylpyridin-3-amineHCID 57875813HCID 57875813、化合物

生成物 1

HCID 44231444HCID 44231444、化合物収率 36.5%

試薬・触媒・溶媒 3

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
10 °C

実験手順

HOBt (40 mg, 0.3 mmol) and DMAP (46 mg, 0.37 mmol) were added to a stirred solution of 3-oxo-3-[4-(3,4,5-trifluoro-benzoyl)-piperazin-1-yl]-propionic acid (83 mg, 0.25 mmol) in DMF (2 mL). The reaction mixture was cooled to 10° C. and EDCI.HCl (58 mg, 0.3 mmol) followed by 6-phenyl-pyridin-3-ylamine (51 mg, 0.3 mmol) were added. The reaction mixture was stirred at room temperature overnight, diluted with water and the product was extracted with ethyl acetate. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated to afford 44 mg (36%) of 3-oxo-N-(6-phenyl-pyridin-3-yl)-3-[4-(3,4,5-trifluoro-benzoyl)-piperazin-1-yl]-propionamide. LCMS: 483.16 (M+1)+, 97.0%, 1H NMR: (DMSO-d6): δ 10.5 (s, 1H), 8.8 (d, 1H), 8.2-8.1 (m, 1H), 8.1 (d, 2H), 8.0 (d, 1H), 7.6-7.4 (m, 5H), 3.4-3.2 (m. 10H).

後処理

  1. additionwere added
  2. extractionthe product was extracted with ethyl acetate
  3. washThe organic layer was washed with brine solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a8fc3171d61f4680bac49d83b8d8ed99
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039463B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート