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Hydrochloric Acid → (3,5-Dibromo-4-methoxy-phenyl)-(7-isoquinolin-4-yl-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl)-methanone

HRID 1943722
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HRID 1943722 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[CH:20]=[N:19][C:14]3[O:15][CH2:16][CH2:17][NH:18][C:13]=3[CH:12]=2)=[CH:3][N:2]=1.[Br:21][C:22]1[CH:23]=[C:24]([CH:28]=[C:29]([Br:33])[C:30]=1[O:31][CH3:32])[C:25](Cl)=[O:26].C(N(CC)CC)C.Cl>ClCCl>[Br:21][C:22]1[CH:23]=[C:24]([C:25]([N:18]2[CH2:17][CH2:16][O:15][C:14]3[N:19]=[CH:20][C:11]([C:4]4[C:5]5[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=5)[CH:1]=[N:2][CH:3]=4)=[CH:12][C:13]2=3)=[O:26])[CH:28]=[C:29]([Br:33])[C:30]=1[O:31][CH3:32]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 337796303,5-Dibromo-4-methoxybenzoyl chlorideHCID 669367327-isoquinolin-4-yl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine

생성물 1

HCID 66936506(3,5-Dibromo-4-methoxy-phenyl)-(7-isoquinolin-4-yl-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl)-methanone수율 23.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Under nitrogen atmosphere, in a 10 ml flask, 7-isoquinolin-4-yl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (22.6 mg, 0.085 mmol) and 3,5-dibromo-4-methoxy-benzoyl chloride (42.2 mg, 0.129 mmol) were dissolved in dichloromethane (1.0 ml). After cooling to 0□, triethylamine (0.06 ml, 0.429 mmol) was added thereto at room temperature for 3 hours. After neutralizing with 1N hydrochloric acid solution, the mixture was extracted with dichloromethane, and the combined organic layer was dried over anhydrous magnesium sulfate (MgSO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on amine silica eluting with a solvent of ethyl acetate and n-hexane. The fractions containing the product were collected and evaporated to obtain white solid (11.0 mg, 23%).

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane
  3. dry with materialthe combined organic layer was dried over anhydrous magnesium sulfate (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on amine silica eluting with a solvent of ethyl acetate and n-hexane
  7. additionThe fractions containing the product
  8. customwere collected
  9. customevaporated

출처 및 근거

ORD 기록
ord-50720bcc5fb742d4b90cd43bdb71f9a9
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394792B2

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