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Formic Acid → 1-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-1H-imidazo[4,5-c]quinoline

HRID 1043009
ノート
印刷プレビュー

反応式

HRID 1043009 の反応式
[CH3:1][C:2]1[C:6]([C:7]2[CH:16]=[C:15]3[C:10]([C:11]([NH:18][CH2:19]C4C=CC=CC=4)=[C:12]([NH2:17])[CH:13]=[N:14]3)=[CH:9][CH:8]=2)=[C:5]([CH3:26])[O:4][N:3]=1.[CH:27]1[CH:28]=[CH:29][C:30]2N(O)N=N[C:31]=2[CH:32]=1.CCN=C=N[CH2:42][CH2:43][CH2:44]N(C)C.[CH3:48]CN(CC)CC.C(O)=O>C(Cl)Cl.O>[C:43]([C:31]1[CH:30]=[CH:29][CH:28]=[CH:27][C:32]=1[N:18]1[C:11]2[C:10]3[CH:9]=[CH:8][C:7]([C:6]4[C:2]([CH3:1])=[N:3][O:4][C:5]=4[CH3:26])=[CH:16][C:15]=3[N:14]=[CH:13][C:12]=2[N:17]=[CH:19]1)([CH3:44])([CH3:48])[CH3:42]
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 284Formic AcidHCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 672063207-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine2 回

生成物 1

HCID 52934041
1-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-1H-imidazo[4,5-c]quinoline
収率 48.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine (for aq preparation see Intermediate 28, 0.2 g, 0.52 mmol) in DCM (10 ml) were added HOBT (0.081 g, 0.62 mmol), EDCI (0.118 g, 0.62 mmol), Et3N (0.062 g, 0.62 mmol) and formic acid (0.025 g, 0.52 mmol). The reaction mixture was stirred at room temperature overnight, then poured into water and extracted with DCM. The organic phase was washed with water, dried over Na2SO4 and concentrated. The crude solid was re-crystallized from EtOAc to give the title compound as off-white crystals (0.1 g, 48%). M.p: 216° C. 1H NMR (300 MHz, CDCl3, ppm) δ: 9.36 (s, 1H), 8.06 (s, 1H), 8.01 (s, 1H), 7.73 (d, J=7.2 Hz, 1H), 7.56 (dd, J=8.1, 8.1 Hz, 1H), 7.34 (dd, J=7.7, 7.7 Hz, 1H), 7.15-7.06 (m, 2H), 2.36 (s, 3H), 2.23 (s, 3H), 1.07 (s, 9H). LC-HRMS: ES+ exact mass calculated for C25H24N4O: 397.2028 MH+, found: 397.2021, Rt 3.03 min.

後処理

  1. extractionextracted with DCM
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customThe crude solid was re-crystallized from EtOAc

出典と根拠

ORDレコード
ord-d2bf2ebdc99d4c0885f49984849a8735
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08557984B2

反応ノート

読み込み中…

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