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1-Hydroxybenzotriazole → 3-Bromo-N-((2-methylpyrimidin-5-yl)methyl)-5-(pyrrolidine-1-carbonyl)benzamide

HRID 1845180
ノート
印刷プレビュー

反応式

HRID 1845180 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[O:12])[CH:10]=1)[C:5]([OH:7])=O.Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1.C(N(CC)C(C)C)(C)C.[CH3:49][C:50]1[N:55]=[CH:54][C:53]([CH2:56][NH2:57])=[CH:52][N:51]=1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[O:12])[CH:10]=1)[C:5]([NH:57][CH2:56][C:53]1[CH:52]=[N:51][C:50]([CH3:49])=[N:55][CH:54]=1)=[O:7]
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 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 21294601(2-Methylpyrimidin-5-yl)methanamineHCID 581881193-Bromo-5-(pyrrolidine-1-carbonyl)benzoic acid

生成物 1

HCID 58188007
3-Bromo-N-((2-methylpyrimidin-5-yl)methyl)-5-(pyrrolidine-1-carbonyl)benzamide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

Into a round-bottom flask were charged 3-bromo-5-(pyrrolidine-1-carbonyl)benzoic acid (340 mg, 1.0 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.39 g, 2.0 mmol), 1-hydroxybenzotriazole (0.30 g, 2.2 mmol), N,N-diisopropylethylamine (0.2 g, 1.5 mmol), methylene chloride (10 mL), 4-dimethylaminopyridine (5 mg, 0.04 mmol), and (2-methylpyrimidin-5-yl)methanamine (240 mg, 1.5 mmol). The mixture was stirred at room temperature overnight, and then diluted with CH2Cl2. The separated organic phase was washed with aq. Na2HPO4, brine, and dried over Na2SO4, and concentrated. The residue was purified via flash chromatography to afford the desired product as an oil. LC-MS: 404.8 [M+1]+; 1H NMR (400 MHz, CDCl3): 8.68 (s, 2H), 7.95 (t, J=1.6 Hz, 1H), 7.76 (t, J=1.3 Hz, 1H), 7.74-7.71 (m, 1H), 7.61 (t, J=1.5 Hz, 1H), 4.57 (d, J=5.8 Hz, 2H), 3.56 (t, J=6.8 Hz, 2H), 3.37 (t, J=6.4 Hz, 2H), 2.73 (s, 3H), 1.96-1.89 (m, 4H).

後処理

  1. washThe separated organic phase was washed with aq. Na2HPO4, brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customThe residue was purified via flash chromatography

出典と根拠

ORDレコード
ord-c26ae73c546e4f49bce656cff007db28
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946439B2

反応ノート

読み込み中…

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