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1-(2-Methoxyphenyl)piperazine → HCID 19972545, 화합물

HRID 1452329
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HRID 1452329 반응식
[Cl:1][CH2:2][CH2:3][O:4][CH2:5][C:6]1[C:15]2[O:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[C:12]([CH3:22])[C:11](=[O:23])[C:10]=2[CH:9]=[CH:8][CH:7]=1.[CH3:24][O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[N:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[ClH:1].[ClH:1].[CH3:24][O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[N:32]1[CH2:37][CH2:36][N:35]([CH2:2][CH2:3][O:4][CH2:5][C:6]2[C:15]3[O:14][C:13]([C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)=[C:12]([CH3:22])[C:11](=[O:23])[C:10]=3[CH:9]=[CH:8][CH:7]=2)[CH2:34][CH2:33]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 13461-(2-Methoxyphenyl)piperazineHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 19972767HCID 19972767, 화합물

생성물 1

HCID 19972545HCID 19972545, 화합물수율 153.6%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

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온도
90 °C

실험 절차

A mixture of 4 g of Intermediate XVIII, 2.4 g of 1-(2-methoxyphenyl)piperazine, 1.96 g of potassium iodide and 1.65 g of anhydrous potassium carbonate in 40 ml of anhydrous dimethylformamide was stirred at 90° C. for 7 hours. After cooling to ambient temperature, the mixture was poured into water and extracted with dichloromethane. The combined extracts were washed with aqueous sodium chloride solution, dried on anhydrous sodium sulfate and evaporated to dryness in vacuo. The residue was crystallized from ethyl acetate and the collected crystals were dissolved in ethanol and treated with excess ethanolic hydrogen chloride to give 5.21 g of the title compound, m.p. 199°-201° C.

후처리

  1. temperatureAfter cooling to ambient temperature
  2. extractionextracted with dichloromethane
  3. washThe combined extracts were washed with aqueous sodium chloride solution
  4. dry with materialdried on anhydrous sodium sulfate
  5. customevaporated to dryness in vacuo
  6. customThe residue was crystallized from ethyl acetate
  7. dissolutionthe collected crystals were dissolved in ethanol
  8. additiontreated with excess ethanolic hydrogen chloride

출처 및 근거

ORD 기록
ord-478a9af32f1148ccacbbd2718a27620f
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05605896

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