Potassium Carbonate → HCID 178432777、化合物

HRID 66720

反応式

HRID 66720 の反応式
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3]([NH2:5])=[NH:4].C(=O)([O-])[O-].[K+].[K+].[Cl:14][CH:15]([C:21]([CH3:23])=O)[C:16](OCC)=[O:17]>O>[Cl:14][C:15]1[C:16]([OH:17])=[N:4][C:3]([C:2]([Cl:7])([Cl:6])[Cl:1])=[N:5][C:21]=1[CH3:23]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11858Ethyl 2-chloroacetoacetateHCID 356082,2,2-Trichloroethanimidamide

生成物 1

HCID 178432777HCID 178432777、化合物収率 31%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 30.0 g (0.18 mole) trichloroacetamidine, 25.2 g (0.18 mole) potassium carbonate, 30.3 g (0.18 mole) ethyl 2-chloroacetoacetate, and 300 ml water was stirred 18 hours. The aqueous solution was decanted from heavier tars and acidified with hydrochloric acid. The precipitate that was formed was filtered, washed, and dried to give 14.7 g (31% yield; mp 130°-145° C.) of crude product. An analytical sample recrystallized from cyclohexane had mp 156°-157° C. The structure was confirmed via infrared and elemental analysis.

後処理

  1. customThe aqueous solution was decanted from heavier tars
  2. customThe precipitate that was formed
  3. filtrationwas filtered
  4. washwashed
  5. customdried
  6. customto give 14.7 g (31% yield; mp 130°-145° C.) of crude product
  7. customAn analytical sample recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-7fa793f8618c41de8b007b91799daca8
出典データセット
uspto-grants-1982_08
特許番号
US04343803

関連ノート

読み込み中…