Sodium Hydroxide → 5H-pyrimido-[4,5-b][1,4]oxazin-6-one

HRID 1943725ノート

反応式

HRID 1943725 の反応式
C[O:2][C:3](=O)[CH2:4][O:5][C:6]1[C:11]([N+:12]([O-])=O)=[C:10](Cl)[N:9]=[CH:8][N:7]=1.[Sn](Cl)(Cl)(Cl)Cl.[OH-].[Na+]>Cl>[N:7]1[C:6]2[O:5][CH2:4][C:3](=[O:2])[NH:12][C:11]=2[CH:10]=[N:9][CH:8]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24287Tin tetrachlorideHCID 86650561(6-Chloro-5-nitro-pyrimidin-4-yloxy)-acetic acid methyl ester

生成物 1

HCID 537908135H-pyrimido-[4,5-b][1,4]oxazin-6-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

In a 25 ml flask, (6-chloro-5-nitro-pyrimidin-4-yloxy)-acetic acid methyl ester (280 mg, 1.1 mmol) and tin tetrachloride (849 mg, 4.5 mmol) were dissolved in hydrochloric acid (7 ml) and heated for 1 hour at 80□. The reaction mixture was cooled to room temperature and neutralized by adding 10% sodium hydroxide solution dropwise, and the formed solid was removed by filtration. The filtrate was extracted with ethyl acetate, and the combined organic layer was washed with saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The obtained yellow solid mixture (107 mg) was used in the next step without further purification.

後処理

  1. temperatureheated for 1 hour at 80□
  2. customthe formed solid was removed by filtration
  3. extractionThe filtrate was extracted with ethyl acetate
  4. washthe combined organic layer was washed with saturated saline solution
  5. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe obtained yellow solid mixture (107 mg) was used in the next step without further purification

出典と根拠

ORDレコード
ord-ad2488066abb447b94dc739b108706b8
出典データセット
uspto-grants-2013_03
特許番号
US08394792B2

反応ノート

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