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Triethylamine → HCID 67148094, 화합물

HRID 2219057
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HRID 2219057 반응식
[C:1]([O:9][C:10]1[C:15](=[O:16])[N:14]2[CH2:17][CH2:18][CH2:19][CH:20](Br)[C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C>CN(C=O)C>[C:1]([O:9][C:10]1[C:15](=[O:16])[N:14]2[CH2:17][CH2:18][CH:19]=[CH:20][C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 67147765HCID 67147765, 화합물

생성물 1

HCID 67148094HCID 67148094, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of methyl 3-(benzoyloxy)-9-bromo-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxylate (obtained following Example 2, Step 1) in anhydrous DMF was added triethylamine (2 eq.). The mixture was stirred and heated to 100° C. for 3 h. After cooling to room temperature the mixture was partitioned between 0.1 M HCl and EtOAc. The aq. phase was again extracted with EtOAc and the combined org. phases were dried over sodium sulfate, filtered, concentrated to dryness under vacuum. The crude product so obtained was used in the subsequent step without further purification. An analytical sample of the title compound was obtained by crystallization from methanol. A pale yellow solid was obtained.

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. customwas partitioned between 0.1 M HCl and EtOAc
  3. extractionThe aq. phase was again extracted with EtOAc
  4. dry with materialphases were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under vacuum
  7. customThe crude product so obtained
  8. customwas used in the subsequent step without further purification

출처 및 근거

ORD 기록
ord-2fb119abc75e47b98096244d789ce04e
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07414045B2

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