Potassium Carbonate → 7-(4-p-Tolyl-piperazin-1-ylmethyl)-chromen-2-one

HRID 581708

반응식

HRID 581708 반응식
BrC[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][C:8](=[O:13])[CH:7]=[CH:6]2.Cl.Cl.[C:16]1([CH3:28])[CH:21]=[CH:20][C:19]([N:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)=[CH:18][CH:17]=1.[C:29](=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:16]1([CH3:28])[CH:17]=[CH:18][C:19]([N:22]2[CH2:23][CH2:24][N:25]([CH2:29][C:12]3[CH:11]=[C:10]4[C:5]([CH:6]=[CH:7][C:8](=[O:13])[O:9]4)=[CH:4][CH:3]=3)[CH2:26][CH2:27]2)=[CH:20][CH:21]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 831121-(p-Tolyl)piperazine dihydrochlorideHCID 105141316-Bromomethyl-chromen-2-one

생성물 1

HCID 99495547-(4-p-Tolyl-piperazin-1-ylmethyl)-chromen-2-one수율 64%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 6-bromomethyl coumarin (0.5 g, 2.09 mmol), 4-tolylpiperazine dihydrochloride (0.51 g, 2.53 mmol) and potassium carbonate (2 g, 14.5 mmol) in acetonitrile (100 mL) was heated under reflux for 18 hours. The cooled mixture was filtered and concentrated under vacuum to provide a solid. Recrystallization from ethyl acetate provided the product as plates (0.45 g, 64% yield), mp 154-155° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. filtrationThe cooled mixture was filtered
  4. concentrationconcentrated under vacuum
  5. customto provide a solid
  6. customRecrystallization from ethyl acetate
  7. customprovided the product as plates (0.45 g, 64% yield), mp 154-155° C.

출처 및 근거

ORD 기록
ord-105eb17341314864bb8a29af18a87b74
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922719

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