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

HRID 2116449
ノート
印刷プレビュー

反応式

HRID 2116449 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-2992591711a44dad83bc7fe3ce61f69d
出典データセット
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07439240B2

反応ノート

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