Acetylsalicylic anhydride → HCID 13051192, 화합물

HRID 904814노트

반응식

HRID 904814 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 13051192HCID 13051192, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-af88a6b3519a486b9b73a9dfb7f6e8f2
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420482

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