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Sodium Iodide → Monatepil

HRID 579748
ノート
印刷プレビュー

反応式

HRID 579748 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 752601-(4-Fluorophenyl)piperazineHCID 13656594HCID 13656594、化合物

生成物 1

HCID 60810Monatepil収率 69.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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);

後処理

  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)

出典と根拠

ORDレコード
ord-3b2cc16ad7ae4f22b5df4dc6b8eb9ad2
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04749703

反応ノート

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