Triethylamine → HCID 178503435、化合物

HRID 1809694ノート

反応式

HRID 1809694 の反応式
Cl[C:2]1[N:7]=[C:6]2[NH:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][N:14]=[C:13]([S:17][CH3:18])[N:12]=3)[C:5]2=[CH:4][N:3]=1.[N:19]1([CH2:25][CH2:26][NH2:27])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.C(N(CC)CC)C>CC(O)C>[CH3:18][S:17][C:13]1[N:12]=[C:11]([C:10]2[C:5]3[C:6](=[N:7][C:2]([NH:27][CH2:26][CH2:25][N:19]4[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]4)=[N:3][CH:4]=3)[NH:8][N:9]=2)[CH:16]=[CH:15][N:14]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 33944N-(2-Aminoethyl)piperidineHCID 178503430HCID 178503430、化合物

生成物 1

HCID 178503435HCID 178503435、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a solution of 6-chloro-3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidine (from Example 7 supra) (450 mg, 1.61 mmol) in 2-propanol (40 mL) was added 2-(piperidin-1-yl)ethanamine (227 mg, 1.77 mmol) followed by triethylamine (160 mg, 1.58 mmol). The reaction mixture was stirred at reflux for 15 hours and the solvent was then removed under reduced pressure. The residue was extracted with dichloromethane (3×30 mL), washed with water (5 mL), dried over anhydrous sodium sulfate, filtered and concentrated to afford [3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-(2-piperidin-1-yl-ethyl)-amine. (Yield 411 mg, crude).

後処理

  1. temperatureat reflux for 15 hours
  2. customthe solvent was then removed under reduced pressure
  3. extractionThe residue was extracted with dichloromethane (3×30 mL)
  4. washwashed with water (5 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-2a410327da10461c91507e4020e16958
出典データセット
uspto-grants-2013_01
特許番号
US08362023B2

反応ノート

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