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Morpholine → 4-[6-Chloro-5-nitro-2-(propylthio)pyrimidin-4-yl]morpholine

HRID 2116449
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HRID 2116449 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[C:13]([N+:14]([O-:16])=[O:15])=[C:12](Cl)[N:11]=[C:10]([S:18][CH2:19][CH2:20][CH3:21])[N:9]=1.C(N(CC)C(C)C)(C)C>C(#N)C>[Cl:7][C:8]1[N:9]=[C:10]([S:18][CH2:19][CH2:20][CH3:21])[N:11]=[C:12]([N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)[C:13]=1[N+:14]([O-:16])=[O:15]
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참가 물질

5

반응물 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 222689244,6-Dichloro-5-nitro-2-(propylthio)pyrimidine

생성물 1

HCID 859081644-[6-Chloro-5-nitro-2-(propylthio)pyrimidin-4-yl]morpholine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Morpholine (2.6 g) was added dropwise to a stirred solution of 4,6-dichloro-5-nitro-2-propylthiopyrimidine (8 g) and N,N-diisopropylethylamine (3.85 g) in acetonitrile (70 ml ) at 0° C. After 1 h the solvent was evaporated and the residue partitioned between ethyl acetate and water, the organics dried (MgSO4) and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with 25% ethyl acetate in isohexane. Yield 7.1 g

후처리

  1. customAfter 1 h the solvent was evaporated
  2. customthe residue partitioned between ethyl acetate and water
  3. dry with materialthe organics dried (MgSO4)
  4. customevaporated under reduced pressure
  5. customThe residue was purified by chromatography on silica eluting with 25% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-2992591711a44dad83bc7fe3ce61f69d
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07439240B2

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