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1-Butanol → 2-(4-((2-Amino-4-(butylamino)-6-methylpyrimidin-5-yl)methyl)-3-methoxyphenyl)acetic acid

HRID 2387902
ノート
印刷プレビュー

反応式

HRID 2387902 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:5]([CH2:13][C:14]2[CH:19]=[CH:18]C(CC#N)=C[C:15]=2[O:23][CH3:24])=[C:4]([CH3:25])[N:3]=1.[OH-:26].[K+].[CH2:28]([OH:32])[CH2:29][CH2:30][CH3:31]>>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:5]([CH2:13][C:14]2[CH:19]=[CH:18][C:30]([CH2:29][C:28]([OH:26])=[O:32])=[CH:31][C:15]=2[O:23][CH3:24])=[C:4]([CH3:25])[N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 2631-ButanolHCID 14797Potassium HydroxideHCID 689572822-(4-((2-Amino-4-(butylamino)-6-methylpyrimidin-5-yl)methyl)-3-methoxyphenyl)acetonitrile

生成物 1

HCID 684141782-(4-((2-Amino-4-(butylamino)-6-methylpyrimidin-5-yl)methyl)-3-methoxyphenyl)acetic acid

反応条件

温度
100 °C

実験手順

The product from step (v) (2.1 g) was dissolved in butan-1-ol (20 mL) and aq. 5M KOH (3.71 ml) was added and the mixture was heated at 100° C. for 36 h. The mixture was allowed to cool and the solvent was evaporated under reduced pressure. The residue was diluted with water (5 mL) and the pH adjusted to ˜7 using conc HCl. The resulting precipitate was collected by filtration and the solid was then suspended in MeCN (10 mL) for 10 min. The suspension was filtered and the solid dried under vacuum overnight to give the subtitle compound as a white solid, 2.60 g.

後処理

  1. temperatureto cool
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was diluted with water (5 mL)
  4. filtrationThe resulting precipitate was collected by filtration
  5. filtrationThe suspension was filtered
  6. customthe solid dried under vacuum overnight

出典と根拠

ORDレコード
ord-a2484ea12b854824bb5f7a7c3a9ed104
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268990B2

反応ノート

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