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Diisopropylethylamine → HCID 25226444、化合物

HRID 1675945
ノート
印刷プレビュー

反応式

HRID 1675945 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[N:10][C:11]([N:17]3[CH:21]=[CH:20][C:19]([CH3:22])=[N:18]3)=[C:12]([C:14]([OH:16])=O)[CH:13]=2)[CH:5]=[N:6][CH:7]=1.[CH3:23][N:24]1[C:33]2[C:28](=[CH:29][C:30]([CH2:34][NH2:35])=[CH:31][CH:32]=2)[CH2:27][CH2:26][CH2:25]1.CCCP(O)(O)=O.CCN(C(C)C)C(C)C>C(#N)C>[CH3:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[N:10][C:11]([N:17]3[CH:21]=[CH:20][C:19]([CH3:22])=[N:18]3)=[C:12]([C:14]([NH:35][CH2:34][C:30]3[CH:29]=[C:28]4[C:33](=[CH:32][CH:31]=3)[N:24]([CH3:23])[CH2:25][CH2:26][CH2:27]4)=[O:16])[CH:13]=2)[CH:5]=[N:6][CH:7]=1
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

6

反応物 4

HCID 81531DiisopropylethylamineHCID 204484Propylphosphonic acidHCID 11121721-(1-Methyl-1,2,3,4-tetrahydroquinolin-6-yl)methanamineHCID 58539042HCID 58539042、化合物

生成物 1

HCID 25226444HCID 25226444、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

To a solution of 5′-methyl-6-(3-methyl-1H-pyrazol-1-yl)-3,3′-bipyridine-5-carboxylic acid (5-2, 0.025 g, 0.085 mmol) and 1-(1-methyl-1,2,3,4-tetrahydroquinolin-6-yl)methanamine (0.015 g, 0.085 mmol) in ACN (0.85 mL) was added 1-propylphosphonic acid cyclic anhydride (T3P, 0.15 mL, 0.255 mmol) followed by Hunig's base (0.089 mL, 0.51 mmol) and the system was stirred at 40° C. for 1 h in an oil bath. The reaction mixture was cooled and partitioned between EtOAc and water, washed with saturated sodium bicarbonate and dried over magnesium sulfate. The reaction mixture was filtered, concentrated and purified via normal phase chromatography (0→10% MeOH in EtOAc) to afford the title compound (5-3) as a bone powder. 1H NMR (500 MHz, CDCl3) δ 8.68 (m, 1H), 8.51 (m, 1H), 8.29 (m, 1H), 8.22 (m, 1H), 7.72 (m, 1H), 7.12 (m, 1H), 7.0 (m, 1H), 6.90 (m, 1H), 6.54 (m, 1H), 6.27 (m, 1H), 4.46 (m, 2H), 3.22(m, 2H), 2.88 (s, 3H), 2.74 (m, 2H), 2.44 (s, 3H), 2.28 (s, 3H), 1.97 (m, 2H). HRMS [M+H] C27H28N6O calc'd 453.2391, found 453.2397.

後処理

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between EtOAc and water
  3. washwashed with saturated sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe reaction mixture was filtered
  6. concentrationconcentrated
  7. custompurified via normal phase chromatography (0→10% MeOH in EtOAc)

出典と根拠

ORDレコード
ord-6d08999fe95d4d08b890d76d14e8e4d4
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08003797B2

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