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Water → 5-Chloro-4,6-dimorpholino-2-(4-phenylpiperazin-1-yl)pyrimidine

HRID 1044654
ノート
印刷プレビュー

反応式

HRID 1044654 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[C:11]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[N:10]=[C:9]([N:19]3[CH2:24][CH2:23][N:22]([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[CH2:21][CH2:20]3)[N:8]=2)[CH2:3][CH2:2]1.[Cl:31]N1C(=O)CCC1=O.O>C(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:31][C:12]1[C:7]([N:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)=[N:8][C:9]([N:19]2[CH2:20][CH2:21][N:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:23][CH2:24]2)=[N:10][C:11]=1[N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 31398ChlorosuccinimideHCID 442504374,6-Dimorpholino-2-(4-phenylpiperazin-1-yl)pyrimidine

生成物 1

HCID 442513235-Chloro-4,6-dimorpholino-2-(4-phenylpiperazin-1-yl)pyrimidine収率 46%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒
HCID 6212
Chloroform
溶媒

実験手順

The synthesis method shall be explained concretely, and in order, below. 4,6-dimorpholino-2-(4-phenylpiperazin-1-yl)pyrimidine (300 mg, 0.73 mmol) was dissolved in chloroform solution (5 ml), benzoyl peroxide (0.3 mg, 0.0014 mmol) and N-chlorosuccinimide (117 mg, 0.87 mmol) was added, and refluxed under heating for 1 hour. Water was added, and extraction was done with dichloromethane. After washing the organic layer with saturated saline, drying was done with MgSO4, and the solvent was distilled away under reduced pressure. Purification was done by silica gel chromatography (hexane:ethyl acetate=4:1), and 142 mg of 5-chloro-4,6-dimorpholino-2-(4-phenylpiperazin-1-yl)pyrimidine was obtained (yield 46%). The melting point measurement result, the MS measurement result, and the NMR data for the obtained Compound 130 are shown below.

後処理

  1. customThe synthesis method
  2. temperaturerefluxed
  3. temperatureunder heating for 1 hour
  4. extractionextraction
  5. washAfter washing the organic layer with saturated saline
  6. customdrying
  7. distillationthe solvent was distilled away under reduced pressure
  8. customPurification

出典と根拠

ORDレコード
ord-3d3ce296a70b40cfa29cb59e45f92637
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563715B2

反応ノート

読み込み中…

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