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Diisopropylethylamine → 3-{2-[4-(6-Fluoro-1,2-benzoxazol-3-yl)piperidin-1-yl]ethyl}-2-methyl-7,8-dihydro-4H-pyrido[1,2-a]pyrimidine-4,9(6H)-dione

HRID 448541
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인쇄 미리보기

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HRID 448541 반응식
[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.Cl[CH2:18][CH2:19][C:20]1[C:25](=[O:26])[N:24]2[CH2:27][CH2:28][CH2:29][C:30](=[O:31])[C:23]2=[N:22][C:21]=1[CH3:32].C(N(C(C)C)CC)(C)C>CO>[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:10][CH2:11][N:12]([CH2:18][CH2:19][C:20]4[C:25](=[O:26])[N:24]5[CH2:27][CH2:28][CH2:29][C:30](=[O:31])[C:23]5=[N:22][C:21]=4[CH3:32])[CH2:13][CH2:14]3)=[N:7][O:8][C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 8494213-(4-Piperidyl)-6-fluoro-1,2-benzisoxazoleHCID 44602516HCID 44602516, 화합물

생성물 1

HCID 446083593-{2-[4-(6-Fluoro-1,2-benzoxazol-3-yl)piperidin-1-yl]ethyl}-2-methyl-7,8-dihydro-4H-pyrido[1,2-a]pyrimidine-4,9(6H)-dione

시약·촉매·용매 1

HCID 887Methanol용매

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온도
26 °C

실험 절차

To the solution of 6-fluoro-3-(piperidin-4-yl)benzo[d]isoxazole (formula-8) (0.62 grams) taken in methanol added 3-(2-chloroethyl)-9-oxo-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one (formula-9) (0.94 grams), diisopropyl ethyl amine (0.75 grams) and refluxed the reaction for 23 hrs. Cooled the reaction mixture to 26° C. and stirred for 15 minutes. Filtered the precipitated solid. Washed the solid with chilled methanol and dried. Separated the compound with column chromatography using chloroform/methanol as an eluent.

후처리

  1. temperaturerefluxed
  2. customthe reaction for 23 hrs
  3. filtrationFiltered the precipitated solid
  4. washWashed the solid with chilled methanol
  5. customdried
  6. customSeparated the compound with column chromatography

출처 및 근거

ORD 기록
ord-94502c24d614460883a677b03f9f20e2
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481729B2

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