Chloroacetyl chloride → Ethyl alpha-methoxyimino-alpha-[2-(chloroacetamido)thiazol-4-yl]acetate

HRID 979683ノート

反応式

HRID 979683 の反応式
[CH3:1][O:2][N:3]=[C:4]([C:10]1[N:11]=[C:12]([NH2:15])[S:13][CH:14]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6].[Cl:16][CH2:17][C:18](Cl)=[O:19]>CC(N(C)C)=O>[CH3:1][O:2][N:3]=[C:4]([C:10]1[N:11]=[C:12]([NH:15][C:18](=[O:19])[CH2:17][Cl:16])[S:13][CH:14]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6]

参加物

4

反応物 2

HCID 6577Chloroacetyl chlorideHCID 581091Ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate

生成物 1

HCID 3593442Ethyl alpha-methoxyimino-alpha-[2-(chloroacetamido)thiazol-4-yl]acetate収率 94.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 10 g of ethyl α-methoxyimino-α-(2-aminothiazol-4-yl)acetate in 100 ml of dimethylacetamide is dropwise added 5.91 g of chloroacetyl chloride under ice-cooling. After the stirring for 1 hour at room temperature, the reaction mixture is poured into ice-water and the resultant solution is extracted with ethyl acetate. The organic layer is washed and dried, followed by the distillation of solvent to give 12.66 g of ethyl α-methoxyimino-α-[2-(chloroacetamido)thiazol-4-yl]acetate as a crystal.

後処理

  1. temperaturecooling
  2. extractionthe resultant solution is extracted with ethyl acetate
  3. washThe organic layer is washed
  4. customdried
  5. distillationfollowed by the distillation of solvent

出典と根拠

ORDレコード
ord-a65774b8a8e34d6aad476565be5f41d1
出典データセット
uspto-grants-1987_05
特許番号
US04668783

反応ノート

読み込み中…