Water → HCID 44608067, 화합물

HRID 1943659노트

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HRID 1943659 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:12]=[N:11][C:6]2[O:7][CH2:8][CH2:9][NH:10][C:5]=2[CH:4]=1.[Br:15][C:16]1[CH:17]=[C:18]([CH:22]=[C:23]([Br:27])[C:24]=1[O:25][CH3:26])[C:19](Cl)=[O:20].C(N(CC)CC)C.O>ClCCl>[Br:15][C:16]1[CH:17]=[C:18]([C:19]([N:10]2[CH2:9][CH2:8][O:7][C:6]3[N:11]=[CH:12][C:3]([C:2]([F:13])([F:1])[F:14])=[CH:4][C:5]2=3)=[O:20])[CH:22]=[C:23]([Br:27])[C:24]=1[O:25][CH3:26]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 337796303,5-Dibromo-4-methoxybenzoyl chlorideHCID 669366917-Trifluoromethyl-2,3-dihydro-1H-pyrido[2,3-B][1,4]oxazine

생성물 1

HCID 44608067HCID 44608067, 화합물수율 98%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a 5 ml flask, 7-trifluoromethyl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (27 mg, 0.23 mmol) and 3,5-dibromo-4-methoxy-benzoyl chloride (65 mg, 0.20 mmol) were dissolved in dichloromethane (0.6 ml), and then triethylamine (0.55 ml, 0.33 mmol) was added thereto dropwise at 0□. After stirring for 4 hours at room temperature, water was added and the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of methanol:dichloromethane=1:100. The fractions containing the product were collected and evaporated to obtain white solid (64 mg, 98%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography on silica eluting with a solvent of methanol
  6. additionThe fractions containing the product
  7. customwere collected
  8. customevaporated

출처 및 근거

ORD 기록
ord-35914bf01d7b47eb9e6e2d6f3352906a
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394792B2

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