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Chloro-N,N-dimethylformiminium chloride → (4-Isopropyl-piperazin-1-yl)-(5-piperidin-1-ylmethylfuran-2-yl)-methanone

HRID 33744
ノート
印刷プレビュー

反応式

HRID 33744 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[O:16][C:15]([CH:17]=O)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH3:19][N+:20]([CH3:23])=CCl.[Cl-].[CH:25]([C:27]1OC(C(O)=O)=C[CH:28]=1)=O.Cl.Cl.C(N1CCNCC1)(C)C>C(Cl)Cl>[CH:1]([N:4]1[CH2:5][CH2:6][N:7]([C:10]([C:12]2[O:16][C:15]([CH2:17][N:20]3[CH2:23][CH2:28][CH2:27][CH2:25][CH2:19]3)=[CH:14][CH:13]=2)=[O:11])[CH2:8][CH2:9]1)([CH3:2])[CH3:3]
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 77311Chloro-N,N-dimethylformiminium chlorideHCID 27937195-Formyl-2-furancarboxylic AcidHCID 122683781-Isopropylpiperazine dihydrochlorideHCID 445160935-(4-Isopropyl-piperazine-1-carbonyl)-furan-2-carbaldehyde

生成物 1

HCID 11244101(4-Isopropyl-piperazin-1-yl)-(5-piperidin-1-ylmethylfuran-2-yl)-methanone収率 87%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

5-(4-Isopropyl-piperazine-1-carbonyl)-furan-2-carbaldehyde. Vilsmeier reagent [(chloromethylene)dimethylammonium chloride, 0.820 g, 6.43 mmol] was suspended in DCM (30 mL) under nitrogen with stirring and cooled to 0° C. To this suspension was added 5-formyl-2-furancarboxylic acid (0.900 g, 6.43 mmol) and the combined mixture was stirred at 0° C. for 30 min. The mixture was warmed to rt, stirred for another 1.5 h, and filtered. The filtrate (containing 5-formyl-furan-2-carbonyl chloride) was set aside and maintained at 0° C. In a second flask, 1-isopropyl-piperizine dihydrochloride (1.28 g, 6.37 mmol) in DCM (15 mL) was cooled to 0° C. The solution was treated with TEA (2.250 g, 22.30 mmol) slowly and then was warmed to rt and stirred for 30 min. The reaction mixture was filtered and the filtrate was cooled to 0° C. This second filtrate was then treated dropwise with the previously prepared solution of 5-formyl-furan-2-carbonyl chloride at 0° C. The combined mixture was stirred at 0° C. for 30 min and then at rt for 1 h. The reaction mixture was cooled to 0° C. and filtered, and the filtrate was washed with H2O (2×15 mL), 0.5 N NaOH (1×15 mL), and satd. aq. NaCl (1×15 mL). The organic layer was separated, dried over anhydrous Na2SO4, filtered, and concentrated to yield the desired product (1.40 g, 87%).

後処理

  1. stirringthe combined mixture was stirred at 0° C. for 30 min
  2. temperatureThe mixture was warmed to rt
  3. stirringstirred for another 1.5 h
  4. filtrationfiltered
  5. additionThe filtrate (containing 5-formyl-furan-2-carbonyl chloride)
  6. temperaturemaintained at 0° C
  7. temperaturewas warmed to rt
  8. stirringstirred for 30 min
  9. filtrationThe reaction mixture was filtered
  10. temperaturethe filtrate was cooled to 0° C
  11. additionThis second filtrate was then treated dropwise with the previously prepared solution of 5-formyl-furan-2-carbonyl chloride at 0° C
  12. stirringThe combined mixture was stirred at 0° C. for 30 min
  13. temperatureThe reaction mixture was cooled to 0° C.
  14. filtrationfiltered
  15. washthe filtrate was washed with H2O (2×15 mL), 0.5 N NaOH (1×15 mL)
  16. customThe organic layer was separated
  17. dry with materialdried over anhydrous Na2SO4
  18. filtrationfiltered
  19. concentrationconcentrated

出典と根拠

ORDレコード
ord-cbc0f986931a440da9f7288fe0833f45
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429659B2

反応ノート

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