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Acetic Acid → HCID 68725159、化合物

HRID 1042276
ノート
印刷プレビュー

反応式

HRID 1042276 の反応式
[CH3:1][O:2][C:3]1[CH:25]=[CH:24][C:6]([CH2:7][N:8]2[CH:16]=[N:15][C:14]3[C:9]2=[N:10][CH:11]=[N:12][C:13]=3[C:17]2[C:18](F)=[N:19][CH:20]=[CH:21][CH:22]=2)=[CH:5][CH:4]=1.[NH2:26][C:27]1[C:28]([CH3:46])=[CH:29][CH:30]=[C:31]2[C:36]=1[N:35]=[CH:34][N:33]=[C:32]2[NH:37][C:38]1[CH:45]=[CH:44][C:41]([C:42]#[N:43])=[CH:40][CH:39]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].CC(O)=O>C1COCC1.CO>[CH3:1][O:2][C:3]1[CH:25]=[CH:24][C:6]([CH2:7][N:8]2[CH:16]=[N:15][C:14]3[C:9]2=[N:10][CH:11]=[N:12][C:13]=3[C:17]2[C:18]([NH:26][C:27]3[C:28]([CH3:46])=[CH:29][CH:30]=[C:31]4[C:36]=3[N:35]=[CH:34][N:33]=[C:32]4[NH:37][C:38]3[CH:45]=[CH:44][C:41]([C:42]#[N:43])=[CH:40][CH:39]=3)=[N:19][CH:20]=[CH:21][CH:22]=2)=[CH:5][CH:4]=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 176Acetic AcidHCID 2733832Lithium HexamethyldisilazideHCID 59627379HCID 59627379、化合物HCID 687253434-(8-Amino-7-methylquinazolin-4-ylamino)benzonitrile

生成物 1

HCID 68725159HCID 68725159、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
140 °C

実験手順

A mixture of 9-(4-methoxybenzyl)-6-(2-fluoropyridin-3-yl)-9H-purine (146 mg, 436 μmol) and 4-(8-amino-7-methylquinazolin-4-ylamino)benzonitrile (120 mg, 436 μmol) in THF (4 mL) was sonicated until all solids became a fine powder. Lithium bis(trimethylsilyl)amide (1.0 M solution in THF; 1.53 mL, 1.53 mmol) was added dropwise with stirring (all solids dissolved and then some solid appeared again). The mixture was stirred at rt for 10 min and then heated in a microwave at 140° C. for 30 min. The mixture was poured into AcOH (0.5 mL) in MeOH (20 mL) and the mixture was stirred for 10 min. Solvent was removed and the product was purified by flash chromatography eluting with MeOH/DCM (2-5%) to give 4-(8-(3-(9-(4-methoxybenzyl)-9H-purin-6-yl)pyridin-2-ylamino)-7-methylquinazolin-4-ylamino)benzonitrile. MS (ESI, pos. ion) m/z: 591.2 [M+H]+

後処理

  1. customwas sonicated until all solids
  2. dissolutiondissolved
  3. stirringThe mixture was stirred at rt for 10 min
  4. stirringthe mixture was stirred for 10 min
  5. customSolvent was removed
  6. customthe product was purified by flash chromatography
  7. washeluting with MeOH/DCM (2-5%)

出典と根拠

ORDレコード
ord-d6186c49083d4cb69ddb6d342b6a411f
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08557830B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート