Hydrochloric Acid → 1-(2-Chloropyrimidin-5-yl)ethan-1-one

HRID 1046097ノート

反応式

HRID 1046097 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([O:10]CC)=[CH2:9])=[CH:4][N:3]=1.Cl>C1COCC1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 143210022-Chloro-5-(1-ethoxyvinyl)pyrimidine

生成物 1

HCID 137157421-(2-Chloropyrimidin-5-yl)ethan-1-one収率 90.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-chloro-5-(1-ethoxyvinyl)pyrimidine (350 mg, 1.9 mmol) in THF (15 mL) was, added aqueous HCl (1N, 15 mL). The mixture was stirred at rt for 4 h, extracted with EtOAc. The organic phase was washed with satd aq NaHCO3 and brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated to give the crude product, which was purified by prep TLC (PE:EA 3:1) to give 1-(2-chloropyrimidin-5-yl)ethanone (268 mg, yield 90%).

後処理

  1. extractionextracted with EtOAc
  2. washThe organic phase was washed with satd aq NaHCO3 and brine
  3. dry with materialThe combined organic layer was dried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customto give the crude product, which
  6. customwas purified by prep TLC (PE:EA 3:1)

出典と根拠

ORDレコード
ord-b0a1778b1c8147f29f11d304aa62e664
出典データセット
uspto-grants-2013_10
特許番号
US08569292B2

反応ノート

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