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Sodium Bicarbonate → 4-(4-fluorobenzoyl)-1-[3-(2-methylthio-10H-phenothiazin-10-yl)propyl]piperidine

HRID 1193985
ノート
印刷プレビュー

反応式

HRID 1193985 の反応式
C(=O)(O)[O-].[Na+].[F:6][C:7]1[CH:20]=[CH:19][C:10]([C:11]([CH:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[O:12])=[CH:9][CH:8]=1.Cl[CH2:22][CH2:23][CH2:24][N:25]1[C:38]2[CH:37]=[C:36]([S:39][CH3:40])[CH:35]=[CH:34][C:33]=2[S:32][C:31]2[C:26]1=[CH:27][CH:28]=[CH:29][CH:30]=2>CN(C)C=O>[F:6][C:7]1[CH:8]=[CH:9][C:10]([C:11]([CH:13]2[CH2:18][CH2:17][N:16]([CH2:22][CH2:23][CH2:24][N:25]3[C:38]4[CH:37]=[C:36]([S:39][CH3:40])[CH:35]=[CH:34][C:33]=4[S:32][C:31]4[C:26]3=[CH:27][CH:28]=[CH:29][CH:30]=4)[CH2:15][CH2:14]2)=[O:12])=[CH:19][CH:20]=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

5

反応物 3

HCID 516892Sodium BicarbonateHCID 27244404-(4-Fluorobenzoyl)piperidineHCID 143914902-Methylthio-10-(3-chloropropyl)-phenothiazine

生成物 1

HCID 143914914-(4-fluorobenzoyl)-1-[3-(2-methylthio-10H-phenothiazin-10-yl)propyl]piperidine収率 50%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
78 °C

実験手順

To a stirred solution of sodium bicarbonate (10 g) in 40 ml of dimethylformamide was added 2.5 g of 4-(4-fluorobenzoyl)piperidine in 40 ml of dimethylformamide, and 4.5 g of 10-(3-chloropropyl)-2-methylthiophenothiazine in 20 ml of dimethylformamide. The reaction mixture was stirred at 78° C. for four hours, cooled, and filtered. The filtrate was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, filtred and concentrated to an oil. The oil was purified by high pressure liquid chromatography on a silica gel column, utilizing ethyl acetate as the eluent. Concentration of the appropriate fractions yielded 2.97 g (36%) of 4-(4-fluorobenzoyl)-1-[3-(2-methylthio-10H-phenothiazin-10-yl)propyl]piperidine as an oil.

後処理

  1. temperaturecooled
  2. filtrationfiltered
  3. additionThe filtrate was poured into water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated to an oil
  8. customThe oil was purified by high pressure liquid chromatography on a silica gel column

出典と根拠

ORDレコード
ord-f29eb838265d49318496d63d720be671
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04812456

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート