Water → HCID 19972518, 화합물

HRID 1452318

반응식

HRID 1452318 반응식
[C:1]([C:4]1[C:13]2[O:12][C:11]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[C:10]([CH3:20])[C:9](=[O:21])[C:8]=2[CH:7]=[CH:6][CH:5]=1)([OH:3])=[O:2].C(=O)([O-])[O-].[K+].[K+].[Cl:28][CH2:29][CH2:30][CH2:31][N:32]1[CH2:37][CH2:36][N:35]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=2[O:44][CH3:45])[CH2:34][CH2:33]1.O>CN(C)C=O>[ClH:28].[ClH:28].[CH3:45][O:44][C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][C:38]=1[N:35]1[CH2:34][CH2:33][N:32]([CH2:31][CH2:30][CH2:29][O:2][C:1]([C:4]2[C:13]3[O:12][C:11]([C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=4)=[C:10]([CH3:20])[C:9](=[O:21])[C:8]=3[CH:7]=[CH:6][CH:5]=2)=[O:3])[CH2:37][CH2:36]1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 770163-Methylflavone-8-carboxylic acidHCID 6226691-(3-Chloropropyl)-4-(2-methoxyphenyl)piperazine

생성물 1

HCID 19972518HCID 19972518, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 4.24 g of 8-carboxy-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran and 6.3 g of anhydrous potassium carbonate in 60 ml of dimethylformamide was stirred at 80° C. for 30 minutes. 5.23 g of 1-(3-chloropropyl)-4-(2-methoxyphenyl)-piperazine was then added and stirring was continued at 80° C. for 3.5 hours. The reaction mixture was cooled to ambient temperature, poured on to iced water and extracted with ethyl acetate. The organic extracts were washed with aqueous sodium chloride solution, dried on anhydrous sodium sulfate, and evaporated to dryness in vacuo. The residue was taken up in ethanol and excess ethanolic hydrogen chloride was added to the solution. Yield: 8.16 g of the title compound, m.p. 198°-203° C.

후처리

  1. stirringstirring
  2. waitwas continued at 80° C. for 3.5 hours
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. extractionextracted with ethyl acetate
  5. washThe organic extracts were washed with aqueous sodium chloride solution
  6. dry with materialdried on anhydrous sodium sulfate
  7. customevaporated to dryness in vacuo
  8. additionexcess ethanolic hydrogen chloride was added to the solution

출처 및 근거

ORD 기록
ord-2e4fa8d28f9d4926887f7aec3539bd5e
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05605896

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