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Sodium Iodide → Monatepil

HRID 579748
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HRID 579748 반응식
Cl[CH2:2][CH2:3][CH2:4][C:5]([NH:7][CH:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][S:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2)=[O:6].[F:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]2)=[CH:26][CH:25]=1.[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:23][C:24]1[CH:25]=[CH:26][C:27]([N:30]2[CH2:35][CH2:34][N:33]([CH2:2][CH2:3][CH2:4][C:5]([NH:7][CH:8]3[C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=4[CH2:12][S:11][C:10]4[CH:19]=[CH:20][CH:21]=[CH:22][C:9]3=4)=[O:6])[CH2:32][CH2:31]2)=[CH:28][CH:29]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 752601-(4-Fluorophenyl)piperazineHCID 13656594HCID 13656594, 화합물

생성물 1

HCID 60810Monatepil수율 69.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

A mixture of 5.0 g of 11-(4-chlorobutyrylamino)-6,11-dihydrodibenzo[b,e]thiepin, 5.5 g of 1-(4-fluorophenyl)piperazine, 5.0 g of sodium iodide and 50 ml of dimethylformamide is stirred at 100° C. for 1.5 hours. After the reaction mixture is cooled to room temperature, 100 ml of 10% aqueous potassium carbonate solution is added and the solution is extracted with three 300-ml portions of chloroform. The combined extracts are washed successively with water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate, and the chloroform is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (100:3) to give 5.0 g of the title compound. m.p. 194°-194.5° C. (recrystallized from chloroform-n-hexane);

후처리

  1. temperatureAfter the reaction mixture is cooled to room temperature
  2. extractionthe solution is extracted with three 300-ml portions of chloroform
  3. washThe combined extracts are washed successively with water and saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. distillationthe chloroform is distilled off
  6. customThe residue is chromatographed on silica gel with chloroform-methanol (100:3)

출처 및 근거

ORD 기록
ord-3b2cc16ad7ae4f22b5df4dc6b8eb9ad2
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04749703

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