Water → 2-[[(2,3-Difluorophenyl)methyl]sulfonyl]-4-[[-2-hydroxy-1-hydroxymethylethyl]amino]-7(8H)-pteridinone

HRID 2105158ノート

反応式

HRID 2105158 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:20]=[C:19]([NH:21][CH:22]([CH2:25][OH:26])[CH2:23][OH:24])[C:18]2[N:17]=[CH:16][C:15](=[O:27])[NH:14][C:13]=2[N:12]=1.[OH2:28].[OH:29]OS([O-])=O.[K+]>C(#N)C>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10]([C:11]1[N:20]=[C:19]([NH:21][CH:22]([CH2:25][OH:26])[CH2:23][OH:24])[C:18]2[N:17]=[CH:16][C:15](=[O:27])[NH:14][C:13]=2[N:12]=1)(=[O:29])=[O:28]

参加物

5

反応物 3

HCID 962WaterHCID 225059782-[[(2,3-Difluorophenyl)methyl]thio]4-[[2-hydroxy-1-(hydroxymethyl)ethyl]amino]-7(8H)-pteridinoneHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 225059372-[[(2,3-Difluorophenyl)methyl]sulfonyl]-4-[[-2-hydroxy-1-hydroxymethylethyl]amino]-7(8H)-pteridinone

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-[[(2,3-Difluorophenyl)methyl]thio]-4-[[-2-hydroxy-1-hydroxymethylethyl]amino]-7(8H)-pteridinone (2.25 g) was stirred in acetonitrile (750 ml) and water (750 ml) with oxone (22.5 g) for 18 hrs. Acetonitrile was removed in vacuo to leave an aqueous suspension. The mixture was extracted into ethyl acetate. The combined extracts were washed with saturated sodium chloride solution, dried (MgSO4) and the solvent removed in vacuo to afford the subtitled compound (1.92 g).

後処理

  1. customAcetonitrile was removed in vacuo
  2. customto leave an aqueous suspension
  3. extractionThe mixture was extracted into ethyl acetate
  4. washThe combined extracts were washed with saturated sodium chloride solution
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-2d8fe9402e314207a48ae185f8f324bb
出典データセット
uspto-grants-2009_08
特許番号
US07579342B2

反応ノート

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