Acetylsalicylic anhydride → HCID 13051192、化合物

HRID 904814ノート

反応式

HRID 904814 の反応式
C(OC1[C:6](=CC=CC=1)[C:7]([O:9][C:10](=[O:21])[C:11]1[C:12](=[CH:17][CH:18]=[CH:19][CH:20]=1)[O:13][C:14](=[O:16])[CH3:15])=O)(=O)C.OC(C)[CH2:28][N:29]1[CH2:34][CH2:33][N:32]([CH2:35][CH:36]([OH:38])[CH3:37])[CH2:31][CH2:30]1>C(OCC)(=O)C>[C:14]([O:13][C:12]1[C:11](=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]([O:9][CH:7]([CH3:6])[CH2:28][N:29]1[CH2:30][CH2:31][N:32]([CH2:35][CH:36]([O:38][C:10](=[O:9])[C:11]2[C:12](=[CH:17][CH:18]=[CH:19][CH:20]=2)[O:13][C:14](=[O:16])[CH3:15])[CH3:37])[CH2:33][CH2:34]1)=[O:21])(=[O:16])[CH3:15]

参加物

4

反応物 2

HCID 15110Acetylsalicylic anhydrideHCID 966981,1'-(Piperazine-1,4-diyl)di(propan-2-ol)

生成物 1

HCID 13051192HCID 13051192、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Dissolve acetylsalicylic anhydride (17.1 g; 0.05 moles) in an apolar organic solvent represented for example by ethyl acetate; add 1,4-bis-(2-hydroxypropyl)piperazine (5.06 g; 0.025 moles) to the solution, and heat up to the boiling point until the reaction is completed. After cooling at room temperature, wash the reaction mixture with a 5 percent aqueous solution of potassium carbonate, and then with water. Anhydrify the organic phase (K2CO3), filter, and treat it with anhydrous hydrochloric acid dissolved in diethylether causing by this procedure the precipitation of the raw product that, after collection and drying, can be recrystallized from a low molecular weight alcohol.

後処理

  1. washwash the reaction mixture with a 5 percent aqueous solution of potassium carbonate
  2. filtrationAnhydrify the organic phase (K2CO3), filter
  3. additiontreat it with anhydrous hydrochloric acid
  4. dissolutiondissolved in diethylether causing by this procedure
  5. customthe precipitation of the raw product that
  6. customafter collection
  7. customdrying
  8. customcan be recrystallized from a low molecular weight alcohol

出典と根拠

ORDレコード
ord-af88a6b3519a486b9b73a9dfb7f6e8f2
出典データセット
uspto-grants-1983_12
特許番号
US04420482

反応ノート

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