Ketorolac → Ketorolac Tromethamine

HRID 1531415

反応式

HRID 1531415 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([C:7]([C:9]2[N:13]3[CH2:14][CH2:15][CH:16]([C:17]([OH:19])=[O:18])[C:12]3=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:6]=1.[NH2:20][C:21]([CH2:26][OH:27])([CH2:24][OH:25])[CH2:22][OH:23]>CO>[CH:1]1[CH:6]=[CH:5][C:4]([C:7]([C:9]2[N:13]3[CH2:14][CH2:15][CH:16]([C:17]([OH:19])=[O:18])[C:12]3=[CH:11][CH:10]=2)=[O:8])=[CH:3][CH:2]=1.[CH2:22]([OH:23])[C:21]([NH2:20])([CH2:26][OH:27])[CH2:24][OH:25]

参加物

4

反応物 2

HCID 3826KetorolacHCID 6503Tris(hydroxymethyl)aminomethane

生成物 1

HCID 84003Ketorolac Tromethamine収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Ketorolac (25 g) and 11.9 g tromethamine were dissolved in 175 mL methanol. The solution was filtered and the filter washed with 40 mL methanol. The resulting solution was concentrated by vacuum distillation. Ethyl acetate (1×172 mL), (1×200 mL) was added to the solution to precipitate the ketorolac tromethamine; and the solution was cooled to room temperature for two hours, cooled further to 0° C., and filtered. The precipitate was washed with ethyl acetate/methanol (4:1 v/v) and dried under vacuum at a temperature of approximately 65° C., to yield ketorolac tromethamine (35.0 g, 95% yield).

後処理

  1. filtrationThe solution was filtered
  2. washthe filter washed with 40 mL methanol
  3. concentrationThe resulting solution was concentrated by vacuum distillation
  4. additionEthyl acetate (1×172 mL), (1×200 mL) was added to the solution
  5. customto precipitate the ketorolac tromethamine
  6. temperaturecooled further to 0° C.
  7. filtrationfiltered
  8. washThe precipitate was washed with ethyl acetate/methanol (4:1 v/v)
  9. customdried under vacuum at a temperature of approximately 65° C.

出典と根拠

ORDレコード
ord-eece73da234a4fe48d968d5dcac0de43
出典データセット
uspto-grants-2001_03
特許番号
US06197976B1

関連ノート

読み込み中…