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Sodium Hydroxide → HCID 86691785、化合物

HRID 1500767
ノート
印刷プレビュー

反応式

HRID 1500767 の反応式
[N:1]1[N:5]2[CH:6]=[CH:7][N:8]=[CH:9][C:4]2=[C:3]([C:10]2[N:15]=[C:14](O)[CH:13]=[CH:12][N:11]=2)[CH:2]=1.P(Cl)(Cl)([Cl:19])=O.[OH-].[Na+]>C(OCC)(=O)C>[Cl:19][C:14]1[CH:13]=[CH:12][N:11]=[C:10]([C:3]2[CH:2]=[N:1][N:5]3[CH:6]=[CH:7][N:8]=[CH:9][C:4]=23)[N:15]=1
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 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 1785164942-(Pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol

生成物 1

HCID 86691785HCID 86691785、化合物収率 104.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2-(pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol (Preparation 10b, 150 mg, 0.7 mmol) in phosphorous oxychloride (1.42 mL, 15.51 mmol) was heated overnight at 110° C. After cooling to ambient temperature, the reaction mixture was poured with caution onto water and basified by addition of a 2N aqueous sodium hydroxide solution. Ethyl acetate was then added and the organic phase was separated, washed with water and brine, dried (MgSO4), filtered and evaporated under reduced pressure to yield the title compound (170 mg, 87%) as a solid which was used in the next synthetic step without further purification.

後処理

  1. additionthe reaction mixture was poured with caution onto water
  2. customthe organic phase was separated
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-53b0bd57eddd440b8d5e1affed9440a3
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206183B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート