Sodium Bicarbonate → 2-(dimethylamino)-N-(4-(2-(pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)quinolin-7-yl)acetamide

HRID 8259

反応式

HRID 8259 の反応式
[CH3:1][N:2]([CH2:4][C:5](Cl)=[O:6])[CH3:3].[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15]([C:22]2[C:31]3[C:26](=[CH:27][C:28]([NH2:32])=[CH:29][CH:30]=3)[N:25]=[CH:24][CH:23]=2)=[C:16]2[CH2:21][CH2:20][CH2:19][N:17]2[N:18]=1.C(=O)(O)[O-].[Na+]>N1C=CC=CC=1>[CH3:1][N:2]([CH3:3])[CH2:4][C:5]([NH:32][C:28]1[CH:27]=[C:26]2[C:31]([C:22]([C:15]3[C:14]([C:9]4[CH:10]=[CH:11][CH:12]=[CH:13][N:8]=4)=[N:18][N:17]4[CH2:19][CH2:20][CH2:21][C:16]=34)=[CH:23][CH:24]=[N:25]2)=[CH:30][CH:29]=1)=[O:6]

参加物

5

実験手順

A mixture of dimethylamino-acetyl chloride (620.0 mg, 13.33 mmol), 4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinolin-7-ylamine (75 mg, 0.23 mmol), and 4-N,N-dimethylaminopyridine (10.2 mg, 0.09 mmol) in dry pyridine (1 mL) is refluxed for 72 h. The mixture is treated with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer is washed with brine, dried (sodium sulfate), concentrated in vacuo, and the residue chromatographed on SiO2 ((5% to 20% methanol in dichloromethane) to yield a yellow oil, 62.3 mg (67%).

後処理

  1. temperatureis refluxed for 72 h
  2. extractionextracted with ethyl acetate
  3. washThe organic layer is washed with brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo
  6. customthe residue chromatographed on SiO2 ((5% to 20% methanol in dichloromethane)
  7. customto yield a yellow oil, 62.3 mg (67%)

出典と根拠

ORDレコード
ord-e9568a52249c4b2fbdc93d52e5bffe68
出典データセット
uspto-grants-2006_08
特許番号
US07087626B2

関連ノート

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