Chlorosuccinimide → 1-butyl-3-chloro-4-hydroxy-2(1H)-Pyridinone

HRID 889631ノート

反応式

HRID 889631 の反応式
[Cl:1]N1C(=O)CCC1=O.[CH2:9]([N:13]1[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]1=[O:20])[CH2:10][CH2:11][CH3:12].C1(CN2C=CC(O)=CC2=O)CC1>CN(C=O)C>[CH2:9]([N:13]1[CH:18]=[CH:17][C:16]([OH:19])=[C:15]([Cl:1])[C:14]1=[O:20])[CH2:10][CH2:11][CH3:12]

参加物

5

反応物 3

HCID 31398ChlorosuccinimideHCID 594970761-butyl-4-hydroxy-1H-pyridine-2-oneHCID 594970981-(Cyclopropylmethyl)-4-hydroxypyridin-2(1H)-one

生成物 1

HCID 594970741-butyl-3-chloro-4-hydroxy-2(1H)-Pyridinone収率 83%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-Chlorosuccinimide (1.6 g, 11.96 mmol) was added to a solution of 1-butyl-4-hydroxy-1H-pyridine-2-one (2.0 g, 11.96 mmol), which was prepared as described for description D2, in DMF (30 ml). The reaction was stirred at room temperature overnight and then it was concentrated in vacuo. The crude product was purified by column chromatography (silica gel; 0-5% methanol/DCM as eluent) to yield intermediate D3 (2.0 g, 83%).

後処理

  1. customwas prepared
  2. concentrationit was concentrated in vacuo
  3. customThe crude product was purified by column chromatography (silica gel; 0-5% methanol/DCM as eluent)

出典と根拠

ORDレコード
ord-9437f495072445d9b0ad4a886cce61a5
出典データセット
uspto-grants-2012_08
特許番号
US08252937B2

反応ノート

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