3-Hydroxybenzaldehyde → 2-(3-formylphenoxy)acetamide

HRID 639726ノート

反応式

HRID 639726 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].Cl[CH2:11][C:12]([NH2:14])=[O:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH2:14][C:12]([CH2:11][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6])=[O:13]

参加物

5

反応物 3

HCID 1013-HydroxybenzaldehydeHCID 6580ChloroacetamideHCID 11430Potassium Carbonate

生成物 1

HCID 110844662-(3-formylphenoxy)acetamide収率 72.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

To a mixture of 12.21 g of 3-hydroxybenzaldehyde, 14.00 g of 2-chloroacetamide and 60 ml of dimethylformamide was added 20.70 g of potassium carbonate, and this was heated to stir at 90° C. for 2 hours. After cooled to room temperature, insolubles were filtered and the filtrate was concentrated under reduced pressure. The resulting residue was dissolved in tetrahydrofuran by heating. Insolubles were filtered and the filtrate was concentration under reduced pressure. The resulting crude crystals were washed with a mixed solution of tetrahydrofuran and t-butyl methyl ether and dried to obtain 13.05 g of 3-(aminocarbonylmethoxy)benzaldehyde [Compound No. (n)] as a crystal.

後処理

  1. temperaturethis was heated
  2. temperatureAfter cooled to room temperature
  3. filtrationinsolubles were filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. dissolutionThe resulting residue was dissolved in tetrahydrofuran
  6. temperatureby heating
  7. filtrationInsolubles were filtered
  8. concentrationconcentration under reduced pressure
  9. washThe resulting crude crystals were washed with a mixed solution of tetrahydrofuran and t-butyl methyl ether
  10. customdried

出典と根拠

ORDレコード
ord-6644c46d1a3542499f32cf5648ae6866
出典データセット
uspto-grants-2010_04
特許番号
US07691883B2

反応ノート

読み込み中…