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N-[(E)-3-(3-Methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxy-cinnamoyl]morpholine → N-{3-[3-(3-Methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxyphenyl]-propanoyl}morpholine

HRID 1532072
ノート
印刷プレビュー

反応式

HRID 1532072 の反応式
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([C:12]3[CH:13]=[C:14]([CH:25]=[CH:26][C:27]=3[O:28][CH2:29][CH2:30][CH3:31])/[CH:15]=[CH:16]/[C:17]([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[O:18])=[N:6][C:5]=2[N:4]([CH2:32][CH2:33][CH3:34])[N:3]=1>C(O)C.[Pd]>[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([C:12]3[CH:13]=[C:14]([CH2:15][CH2:16][C:17]([N:19]4[CH2:20][CH2:21][O:22][CH2:23][CH2:24]4)=[O:18])[CH:25]=[CH:26][C:27]=3[O:28][CH2:29][CH2:30][CH3:31])=[N:6][C:5]=2[N:4]([CH2:32][CH2:33][CH3:34])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 135532857N-[(E)-3-(3-Methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxy-cinnamoyl]morpholine

生成物 1

HCID 135453502N-{3-[3-(3-Methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxyphenyl]-propanoyl}morpholine収率 74%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of N-[(E)-3-(3-methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxycinnamoyl]morpholine (0.5 g, 0.0011 mol) in ethanol (30 ml) was stirred with 10% palladium on charcoal catalyst (0.05 g) under a hydrogen pressure of 50 p.s.i. (3.45 bar) at room temperature for 14 hours. The reaction mixture was filtered and solvent removed by evaporation under vacuum. Trituration of the residue with diethyl ether, followed by crystallisation from ethyl acetate-hexane, afforded the title compound as white crystals (0.37 g, 74%), m.p. 132-133° C. Found: C, 64.39; H, 7.26; N, 14.80. C25H33N5O4 requires C, 64.22; H, 7.11; N, 14.98%.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customsolvent removed by evaporation under vacuum
  3. customTrituration of the residue with diethyl ether, followed by crystallisation from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-b30fcd3774e14f878d48834b67695762
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06200980B1

反応ノート

読み込み中…

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