Water → 4-(7-Azaindol-5-yloxy)-6-hydroxy-7-methoxyquinazohne

HRID 2068031ノート

反応式

HRID 2068031 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([O:10][C:11]3[C:20]4[C:15](=[CH:16][C:17]([O:29][CH3:30])=[C:18]([O:21]CC5C=CC=CC=5)[CH:19]=4)[N:14]=[CH:13][N:12]=3)=[CH:7][N:8]=2)[CH:3]=[CH:2]1.C([O-])=O.[NH4+].O>[Pd].CN(C=O)C>[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([O:10][C:11]3[C:20]4[C:15](=[CH:16][C:17]([O:29][CH3:30])=[C:18]([OH:21])[CH:19]=4)[N:14]=[CH:13][N:12]=3)=[CH:7][N:8]=2)[CH:3]=[CH:2]1

参加物

6

反応物 3

HCID 962WaterHCID 2723923Ammonium formateHCID 666467954-(7-Azaindol-5-yloxy)-6-benzyloxy-7-methoxyquinazoline

生成物 1

HCID 589602364-(7-Azaindol-5-yloxy)-6-hydroxy-7-methoxyquinazohne収率 96.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-(7-azaindol-5-yloxy)-6-benzyloxy-7-methoxyquinazoline (0.36 g, 0.873 mmol), ammonium formate (0.55 g, 8.73 mmol) and 10% palladium on carbon (0.05 g) in DMF (7 ml) containing water (0.3 ml) was stirred at ambient temperature for 1 hour. The mixture was filtered and the filtrate was evaporated. The residue was triturated under diethyl ether and the solid was filtered, washed with ether and dried under vacuum. The solid was triturated under water, filtered, washed with water and dried under vacuum over P2O5 to give 4-(7-azaindol-5-yloxy)-6-hydroxy-7-methoxyquinazoline (0.26 g, 85%).

後処理

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated
  3. customThe residue was triturated under diethyl ether
  4. filtrationthe solid was filtered
  5. washwashed with ether
  6. customdried under vacuum
  7. customThe solid was triturated under water
  8. filtrationfiltered
  9. washwashed with water
  10. dry with materialdried under vacuum over P2O5

出典と根拠

ORDレコード
ord-e4eceac8004f4068a9e06d1e737d3e81
出典データセット
uspto-grants-2012_10
特許番号
US08293902B2

反応ノート

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