Methanol → HCID 44608071, 화합물

HRID 1943672노트

반응식

HRID 1943672 반응식
[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

참가 물질

7

반응물 4

HCID 887MethanolHCID 6344DichloromethaneHCID 25134Boron tribromideHCID 86650559HCID 86650559, 화합물

생성물 1

HCID 44608071HCID 44608071, 화합물수율 54%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 63651,1-Dichloroethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-77a1dfff7d904ed8bca5f42ada668eb0
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394792B2

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