Water → HCID 25060062、化合物

HRID 657808ノート

反応式

HRID 657808 の反応式
[Si]([O:8][CH2:9][C@@H:10]([NH:19][C:20]1[C:21]2[CH2:29][N:28]([C:30]3[CH:37]=[CH:36][C:35]([CH3:38])=[CH:34][C:31]=3[C:32]#[N:33])[CH2:27][CH2:26][C:22]=2[N:23]=[CH:24][N:25]=1)[C:11]1[CH:12]=[N:13][C:14]([O:17][CH3:18])=[N:15][CH:16]=1)(C(C)(C)C)(C)C.CCCC[N+](CCCC)(CCCC)CCCC.[F-].O.CCOC(C)=O>C1COCC1>[OH:8][CH2:9][C@@H:10]([NH:19][C:20]1[C:21]2[CH2:29][N:28]([C:30]3[CH:37]=[CH:36][C:35]([CH3:38])=[CH:34][C:31]=3[C:32]#[N:33])[CH2:27][CH2:26][C:22]=2[N:23]=[CH:24][N:25]=1)[C:11]1[CH:16]=[N:15][C:14]([O:17][CH3:18])=[N:13][CH:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 2724141Tetrabutylammonium FluorideHCID 69177701HCID 69177701、化合物

生成物 1

HCID 25060062HCID 25060062、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of (S)-2-(4-(2-(tert-butyldimethylsilyloxy)-1-(methoxypyrimidin5-yl)ethylamino)-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-methylbenzonitrile (740 mg, 1.39 mmol) in THF (10 mL) was added 1M TBAF in THF (5 mL). The reaction mixture was stirred at room temperature for 10 minutes, and then treated with water and EtOAc. The organic layer was washed with aq. NaHCO3 and brine, dried (MgSO4), and concentrated. The residue was purified by semi-preparative HPLC to yield a white solid.

後処理

  1. washThe organic layer was washed with aq. NaHCO3 and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customThe residue was purified by semi-preparative HPLC
  5. customto yield a white solid

出典と根拠

ORDレコード
ord-36f6e397d01a4b77bab4726712777fc3
出典データセット
uspto-grants-2011_12
特許番号
US08076345B2

反応ノート

読み込み中…