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

HRID 581708

反応式

HRID 581708 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-105eb17341314864bb8a29af18a87b74
出典データセット
uspto-grants-1999_07
特許番号
US05922719

関連ノート

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