Water → Ethyl 1-(3-bromophenyl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate

HRID 1294358ノート

反応式

HRID 1294358 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][CH:24]=1)[NH:5][CH:6]=[C:7]([C:13](=[O:21])[C:14]1[CH:19]=[CH:18][CH:17]=[N:16][C:15]=1Cl)[C:8]([O:10][CH2:11][CH3:12])=[O:9].[H-].[Na+].O>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([N:5]2[C:15]3[C:14](=[CH:19][CH:18]=[CH:17][N:16]=3)[C:13](=[O:21])[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6]2)[CH:22]=[CH:23][CH:24]=1

参加物

5

反応物 3

HCID 962WaterHCID 24758Sodium hydrideHCID 178471910HCID 178471910、化合物

生成物 1

HCID 11057804Ethyl 1-(3-bromophenyl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

The crude compound from Step 1 was dissolved in tetrahydrofuran (0.3 M), the solution was cooled to 0° C., and sodium hydride (as a 60% dispersion in oil, 1.3 eq) was added in portions. After stirring at 0° C. for 1 hour, the mixture was allowed to warm up to room temperature. After 2 hours, water was added to the suspension and and the insoluble solid was filtered and washed copiously with water. When dry, the solid was stirred in ether at room temperature for 24 hours and filtered to afford the title compound as a cream-colored solid.

後処理

  1. temperatureto warm up to room temperature
  2. waitAfter 2 hours
  3. filtrationthe insoluble solid was filtered
  4. washwashed copiously with water
  5. customWhen dry
  6. stirringthe solid was stirred in ether at room temperature for 24 hours
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-57caa9857e8341c3a7d8f459e2e78e7b
出典データセット
uspto-grants-2007_07
特許番号
US07238706B2

反応ノート

読み込み中…