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Hydrochloric Acid → HCID 66936726, 화합물

HRID 1943648
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HRID 1943648 반응식
[NH:1]1[CH2:6][CH2:5][O:4][C:3]2[CH:7]=[N:8][CH:9]=[CH:10][C:2]1=2.[Cl:11][C:12]1[CH:13]=[C:14]([CH:18]=[C:19]([N+:23]([O-:25])=[O:24])[C:20]=1[O:21][CH3:22])[C:15](Cl)=[O:16].C(N(CC)CC)C.Cl>ClCCl>[Cl:11][C:12]1[CH:13]=[C:14]([C:15]([N:1]2[CH2:6][CH2:5][O:4][C:3]3[CH:7]=[N:8][CH:9]=[CH:10][C:2]2=3)=[O:16])[CH:18]=[C:19]([N+:23]([O-:25])=[O:24])[C:20]=1[O:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 219615362,3-Dihydro-1H-pyrido[3,4-b][1,4]oxazineHCID 86650557Benzoyl chloride, 3-chloro-4-methoxy-5-nitro-

생성물 1

HCID 66936726HCID 66936726, 화합물수율 81%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a 10 ml flask, 2,3-dihydro-1H-pyrido[3,4-b][1,4]oxazine (57 mg, 0.42 mmol) and 3-chloro-4-methoxy-5-nitro-benzoyl chloride (117 mg, 0.47 mmol) were dissolved in dichloromethane. Triethylamine (0.29 ml, 2.1 mmol) was added thereto and then stirred at room temperature for 2 hours. After neutralizing with 1N hydrochloric acid solution, the reaction mixture was extracted with dichloromethane. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4) and filtered and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica with a solvent of ethyl acetate:n-hexane=1:2. The fractions containing the product were collected and evaporated to obtain yellow solid (118 mg, 81%).

후처리

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

출처 및 근거

ORD 기록
ord-a0be14f68bd6473189dc70f22f199d0d
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394792B2

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