Methanol → HCID 44608071、化合物

HRID 1943672ノート

反応式

HRID 1943672 の反応式
[Cl:1][C:2]1[C:11]2[N:10]([C:12]([C:14]3[CH:19]=[C:18]([Br:20])[C:17]([O:21]C)=[C:16]([Br:23])[CH:15]=3)=[O:13])[CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1.B(Br)(Br)Br.ClCCl.CO>ClC(Cl)C.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:11]2[N:10]([C:12]([C:14]3[CH:15]=[C:16]([Br:23])[C:17]([OH:21])=[C:18]([Br:20])[CH:19]=3)=[O:13])[CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 887MethanolHCID 6344DichloromethaneHCID 25134Boron tribromideHCID 86650559HCID 86650559、化合物

生成物 1

HCID 44608071HCID 44608071、化合物収率 54%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 63651,1-Dichloroethane溶媒

実験手順

In a 5 ml flask equipped with a reflux apparatus, (5-chloro-2,3-dihydro -pyrido[4,3-b][1,4]oxazin-4-yl)-(3,5-dibromo-4-methoxy-phenyl)-methanone (48 mg, 0.1 mmol) was dissolved in dichloroethane (0.5 ml) and chloroform (0.5 ml). 1.0M Boron tribromide dissolved in dichloromethane (1 ml, 1 mmol) was added thereto dropwise at room temperature. The reaction mixture was stirred at 450 for 18 hours. After cooling to room temperature, methanol (1 ml) was added and then stirred at room temperature for 10 minutes. After evaporating under reduced pressure, dichloromethane was added and then stirred. The reaction mixture was filtered to obtain the target compound 30 as white solid (24 mg, 54%).

後処理

  1. additionwas added
  2. customdropwise at room temperature
  3. stirringstirred at room temperature for 10 minutes
  4. customAfter evaporating under reduced pressure, dichloromethane
  5. additionwas added
  6. stirringstirred
  7. filtrationThe reaction mixture was filtered

出典と根拠

ORDレコード
ord-77a1dfff7d904ed8bca5f42ada668eb0
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…