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Cesium carbonate → 7-(3,5-Dimethylisoxazol-4-yl)-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one

HRID 589093
ノート
印刷プレビュー

反応式

HRID 589093 の反応式
Br[C:2]1[CH:11]=[CH:10][C:9]2[NH:12][C:13](=[O:14])[N:7]3[C:8]=2[C:3]=1[CH2:4][CH2:5][CH:6]3[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.BrC1C=C2C3=C(NC(=O)N3C(C3C=CC=CC=3)CC2)C=1.[CH3:41][C:42]1[C:46](B(O)O)=[C:45]([CH3:50])[O:44][N:43]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>COCCOC.O>[CH3:41][C:42]1[C:46]([C:2]2[CH:11]=[CH:10][C:9]3[NH:12][C:13](=[O:14])[N:7]4[C:8]=3[C:3]=2[CH2:4][CH2:5][CH:6]4[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[C:45]([CH3:50])[O:44][N:43]=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

7

反応物 4

HCID 10796Cesium carbonateHCID 27343463,5-Dimethylisoxazole-4-boronic acidHCID 904091427-Bromo-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-oneHCID 904098178-bromo-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one

生成物 1

HCID 904098527-(3,5-Dimethylisoxazol-4-yl)-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one収率 56.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
90 °C

実験手順

A mixture of 7-bromo-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one (0.050 g, 0.15 mmol) (4.4:1 mixture of isomers with 8-bromo-4-phenyl-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one as the minor isomer), (3,5-dimethylisoxazol-4-yl)boronic acid (10.7 mg, 0.0759 mmol), and cesium carbonate (99.0 mg, 0.304 mmol) in 1,2-dimethoxyethane (1.21 mL) and water (0.303 mL) was degassed with nitrogen for 5 min. The reaction mixture was treated with PEPPSI-IPr (5.2 mg, 0.0076 mmol) [Aldrich, cat. #669032], degassed with nitrogen for 5 min, and heated at 90° C. for 1 h. The reaction mixture was then diluted with ethyl acetate (25 mL) and water (20 mL). The organic layer was separated, washed with brine, dried over sodium sulfate, filtered, and concentrated to give a crude residue. Purification via preparative LCMS (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.1% trifluoroacetic acid, at flow rate of 60 mL/min) gave the desired product (14.7 mg, 28%) as a racemic mixture. 1H NMR (500 MHz, CDCl3) δ 10.00 (s, 1H), 7.34-7.20 (m, 3H), 7.08-6.95 (m, 3H), 6.88-6.76 (m, 1H), 5.54 (s, 1H), 2.45-1.96 (m, 10H); LCMS calculated for C21H20N3O2 (M+H)+: m/z=346.2. found: 346.1.

後処理

  1. customwas degassed with nitrogen for 5 min
  2. customdegassed with nitrogen for 5 min
  3. additionThe reaction mixture was then diluted with ethyl acetate (25 mL) and water (20 mL)
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give a crude residue
  10. customPurification via preparative LCMS (XBridge C18 column
  11. washeluting with a gradient of acetonitrile/water containing 0.1% trifluoroacetic acid, at flow rate of 60 mL/min)

出典と根拠

ORDレコード
ord-c4169bb0319d47f59557675aef61d145
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09227985B2

反応ノート

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