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Dimethylformamide → HCID 86614656、化合物

HRID 1983848
ノート
印刷プレビュー

反応式

HRID 1983848 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([Cl:19])=[C:15]([CH3:18])[CH:16]=3)[O:11][C:10](=[O:20])[C:9]=2[CH2:21][C:22]([NH:24][C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=2[C:32]([F:35])([F:34])[F:33])=[O:23])[CH:5]=[CH:6][CH:7]=1.CN(C)C=O.[C:41]([O:45][CH2:46][CH2:47][CH2:48][CH3:49])(=[O:44])[CH:42]=[CH2:43].C([O-])(=O)C.[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.O.C(OCC)(=O)C>[Cl:19][C:14]1[CH:13]=[C:12]2[C:17]([C:8]([C:4]3[CH:3]=[C:2](/[CH:43]=[CH:42]/[C:41]([O:45][CH2:46][CH2:47][CH2:48][CH3:49])=[O:44])[CH:7]=[CH:6][CH:5]=3)=[C:9]([CH2:21][C:22]([NH:24][C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=3[C:32]([F:35])([F:33])[F:34])=[O:23])[C:10](=[O:20])[O:11]2)=[CH:16][C:15]=1[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 6228DimethylformamideHCID 8846Butyl AcrylateHCID 517045Sodium AcetateHCID 54753138HCID 54753138、化合物

生成物 1

HCID 86614656HCID 86614656、化合物収率 84.9%

試薬・触媒・溶媒 4

HCID 80271Tri-o-tolylphosphine
触媒
HCID 167845palladium(II) acetate触媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2-[4-(3-bromophenyl)-7-chloro-6-methyl-2-oxo-2H-chromen-3-yl]-N-[4-fluoro-2-(trifluoromethyl)phenyl]acetamide (2.00 g), palladium acetate (0.0079 g) and tri-o-tolyl phosphine (0.0214 g) was placed in a reaction vessel, and nitrogen was passed through the reaction vessel for 10 minutes to replace the atmosphere of the reaction vessel with nitrogen. N,N-Dimethylformamide (10 ml), butyl acrylate (0.677 g) and sodium acetate (0.317 g) were added successively thereto, and the mixture was stirred at room temperature for about 20 minutes. Then, the mixture was stirred at 110° C. for 3 hours and cooled to room temperature. Ethyl acetate (20 ml) and water (20 ml) were poured to the reaction mixture and, after stirring, an organic layer was separated. The organic layer was washed successively with a mixture of 10% saline (18 ml) and conc. hydrochloric acid (2 ml), and 10% saline (20 ml). Activated charcoal (0.1 g) and tributyl phosphine (0.0712 g) were added to the organic layer, and the mixture was stirred at room temperature for 10 minutes. Then, the activated charcoal was removed by filtration and washed with ethyl acetate (4 ml). The combined filtrate and washings were concentrated to 6.0 g under reduced pressure, and n-heptane (12 ml) was added dropwise to the residue to precipitate crystals. After stirring at 5° C. for 1 hour, the crystals were collected by filtration and washed with cold ethyl acetate/n-heptane (1/3, 4 ml). A mixture of the resulting crystals (2.06 g) and acetone (10 ml) were heated to 50° C. to dissolve the mixture, activated charcoal (0.1 g) was added thereto, and the mixture was stirred for 10 minutes. The activated charcoal was removed by filtration, and washed with acetone (4 ml). Water (4.6 ml) was added dropwise to the combined filtrate and washings, and the mixture was stirred at 5° C. for 1 hour. Crystals were collected by filtration, and washed with cold acetone/water (2/1, 4 ml) to obtain the title compound (1.84 g, yield 84.9%).

後処理

  1. customwas placed in a reaction vessel
  2. stirringThen, the mixture was stirred at 110° C. for 3 hours
  3. temperaturecooled to room temperature
  4. stirringafter stirring
  5. customan organic layer was separated
  6. washThe organic layer was washed successively with a mixture of 10% saline (18 ml) and conc. hydrochloric acid (2 ml), and 10% saline (20 ml)
  7. additionActivated charcoal (0.1 g) and tributyl phosphine (0.0712 g) were added to the organic layer
  8. stirringthe mixture was stirred at room temperature for 10 minutes
  9. customThen, the activated charcoal was removed by filtration
  10. washwashed with ethyl acetate (4 ml)
  11. concentrationThe combined filtrate and washings were concentrated to 6.0 g under reduced pressure, and n-heptane (12 ml)
  12. additionwas added dropwise to the residue
  13. customto precipitate crystals
  14. stirringAfter stirring at 5° C. for 1 hour
  15. filtrationthe crystals were collected by filtration
  16. washwashed with cold ethyl acetate/n-heptane (1/3, 4 ml)
  17. additionA mixture of the resulting crystals (2.06 g) and acetone (10 ml)
  18. temperaturewere heated to 50° C.
  19. dissolutionto dissolve the mixture, activated charcoal (0.1 g)
  20. additionwas added
  21. stirringthe mixture was stirred for 10 minutes
  22. customThe activated charcoal was removed by filtration
  23. washwashed with acetone (4 ml)
  24. additionWater (4.6 ml) was added dropwise to the combined filtrate and washings
  25. stirringthe mixture was stirred at 5° C. for 1 hour
  26. filtrationCrystals were collected by filtration
  27. washwashed with cold acetone/water (2/1, 4 ml)

出典と根拠

ORDレコード
ord-9113f16d1a0442b68ed140c72bcd2d32
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07541478B2

反応ノート

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