Sodium hydride → HCID 86650559, 화합물

HRID 1943671노트

반응식

HRID 1943671 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 86650559HCID 86650559, 화합물수율 50%

시약·촉매·용매 1

HCID 8909Butyl ether용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-f64b2efa4f3943b8a0e4a6f6d37c7a29
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394792B2

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