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Trifluoroacetic anhydride → HCID 118598640, 화합물

HRID 1050404
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HRID 1050404 반응식
[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N+:6]([O-])[CH:7]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:17]>CN(C)C=O>[Br:1][C:2]1[C:3](=[O:17])[NH:4][C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 118599043HCID 118599043, 화합물

생성물 1

HCID 118598640HCID 118598640, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

To a 0° C. cooled solution of 5-bromo-2-(ethoxycarbonyl)pyrimidine 1-oxide (3, 0.62 g, 2.5 mmol) in dimethylformamide (6 mL), trifluoroacetic anhydride (3.1 g, 15 mmol) was added dropwise. The reaction mixture was heated at 50° C. for 18 h. TLC showed consumption of starting material and solvent was removed under reduced pressure. The residue was triturated with methanol (2 mL) and filtered. The solid was washed with diethyl ether and dried under reduced pressure to afford ethyl 5-bromo-6-oxo-1,6-dihydropyrimidine-2-carboxylate (4) as off white solid. Yield: 0.21 g, 34%; MS (ESI) m/z 245.09 [M−1]−.

후처리

  1. additionwas added dropwise
  2. customconsumption of starting material and solvent
  3. customwas removed under reduced pressure
  4. customThe residue was triturated with methanol (2 mL)
  5. filtrationfiltered
  6. washThe solid was washed with diethyl ether
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-cd5cab4f752846e0be421896c13218c7
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382248B2

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