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Dichloromethane → 3-Cyclohexyl-6-{2-methoxy-4-[(4-methyl-1-piperazinyl)sulfonyl]phenyl}-1-methyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one

HRID 915934
ノート
印刷プレビュー

反応式

HRID 915934 の反応式
ClCCl.[CH:4]1([C:10]2[C:18]3[C:17](=[O:19])[NH:16][C:15]([C:20]4[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][C:21]=4[O:30][CH3:31])=[N:14][C:13]=3[N:12]([CH3:32])[N:11]=2)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.[CH3:33][N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1.C(N(CC)CC)C>O>[CH:4]1([C:10]2[C:18]3[C:17](=[O:19])[NH:16][C:15]([C:20]4[CH:25]=[CH:24][C:23]([S:26]([N:37]5[CH2:38][CH2:39][N:34]([CH3:33])[CH2:35][CH2:36]5)(=[O:28])=[O:27])=[CH:22][C:21]=4[O:30][CH3:31])=[N:14][C:13]=3[N:12]([CH3:32])[N:11]=2)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1
参加物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 6344DichloromethaneHCID 8471TriethylamineHCID 531671-MethylpiperazineHCID 1360059474-(3-Cyclohexyl-1-methyl-4-oxo-4,5-dihydro-1H-pyrazolo[3,4-d]pyrimidin-6-yl)-3-methoxybenzenesulfonyl chloride

生成物 1

HCID 1360057943-Cyclohexyl-6-{2-methoxy-4-[(4-methyl-1-piperazinyl)sulfonyl]phenyl}-1-methyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 2 ml anhydrous dichloromethane solution of 87.2 mg (0.2 mmol) of the compound obtained in Example 48, 26.6 μl (0.24 mmol) of N-methylpiperazine and 70 μl (0.5 mmol) of triethylamine were added, and the mixture was stirred at room temperature for 20 hours. Then, water was added to the reaction mixture, and the mixture was extracted with dichloromethane. The organic layer was washed with water and a saturated aqueous solution of sodium chloride. After the washed layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=50/1˜30/1) to obtain 87 mg (87%) of the captioned compound.

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe organic layer was washed with water
  3. dry with materialAfter the washed layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (chloroform/methanol=50/1˜30/1)

出典と根拠

ORDレコード
ord-50bf40bbffae4bb5808c2d6a88d27d24
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07268128B2

反応ノート

読み込み中…

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