Sodium hydride → HCID 86650559、化合物

HRID 1943671ノート

反応式

HRID 1943671 の反応式
[Cl:1][C:2]1[C:11]2[NH:10][CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1.[H-].[Na+].[Br:14][C:15]1[CH:16]=[C:17]([CH:21]=[C:22]([Br:26])[C:23]=1[O:24][CH3:25])[C:18](Cl)=[O:19]>C(OCCCC)CCC>[Cl:1][C:2]1[C:11]2[N:10]([C:18]([C:17]3[CH:21]=[C:22]([Br:26])[C:23]([O:24][CH3:25])=[C:15]([Br:14])[CH:16]=3)=[O:19])[CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 337796303,5-Dibromo-4-methoxybenzoyl chlorideHCID 707007455-Chloro-3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine

生成物 1

HCID 86650559HCID 86650559、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8909Butyl ether溶媒

実験手順

In a 50 ml flask equipped with a reflux apparatus, 5-chloro-3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine (890 mg, 5.22 mmol) was dissolved in butyl ether (20 ml), and 60% sodium hydride in mineral oil (250 mg, 6.26 mmol) was added and stirred at 1250 for 3.5 hours. The mixture was cooled to room temperature and 3,5-dibromo-4-methoxy-benzoyl chloride (2.06 g, 6.26 mmol) was added thereto and then stirred at 1250 for 24 hours. The mixture was cooled to room temperature and filtered and evaporated under reduced pressure. The residue was washed with methanol and dried under reduced pressure to obtain white solid (1.2 g, 50%).

後処理

  1. stirringstirred at 1250 for 24 hours
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. washThe residue was washed with methanol
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-f64b2efa4f3943b8a0e4a6f6d37c7a29
出典データセット
uspto-grants-2013_03
特許番号
US08394792B2

反応ノート

読み込み中…