Sodium Acetate → N-(5-chloropyridin-2-yl)-2-acetoxyacetamide

HRID 1820934

反応式

HRID 1820934 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][N:7]=1)=[O:4].[C:13]([O-:16])(=[O:15])[CH3:14].[Na+]>CN(C)C=O.C(OCC)(=O)C>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[CH2:2][O:16][C:13](=[O:15])[CH3:14])=[N:7][CH:8]=1

参加物

5

反応物 2

HCID 517045Sodium AcetateHCID 51511482-chloro-N-(5-chloropyridin-2-yl)acetamide

生成物 1

HCID 23062652N-(5-chloropyridin-2-yl)-2-acetoxyacetamide収率 89.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

2-Chloro-N-(5-chloropyridin-2-yl)acetamide (30.68 g) obtained in Reference Example 26(1) is dissolved in N,N-dimethylformamide (500 ml), thereto is added sodium acetate (24.55 g), and the mixture is stirred at 60° C. for 5 hours. The reaction solution is diluted with ethyl acetate, washed successively with water and saturated brine. The solution is dried over magnesium sulfate, treated with activated charcoal, and the filtrate is concentrated under reduced pressure. The resulting residue is suspended in n-hexane and crystals are collected by filtration, washed with n-hexane, and dried to give N-(5-chloropyridin-2-yl)-2-acetoxyacetamide (30.58 g). APCI-MS M/Z:229/231[M+H]+

後処理

  1. washwashed successively with water and saturated brine
  2. dry with materialThe solution is dried over magnesium sulfate
  3. additiontreated with activated charcoal
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. filtrationcrystals are collected by filtration
  6. washwashed with n-hexane
  7. customdried

出典と根拠

ORDレコード
ord-69929170c9814fa581953b4d1a5fee46
出典データセット
uspto-grants-2009_10
特許番号
US07605158B2

関連ノート

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