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Acetic Acid → HCID 57787267、化合物

HRID 2426783
ノート
印刷プレビュー

反応式

HRID 2426783 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][N:7]2[C:11](=[O:12])[NH:10][C:9](=[O:13])[O:8]2)=[CH:4][CH:3]=1.[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([CH:29]=O)[CH:24]=2)=[C:19]([CH3:31])[CH:18]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+:49]>C1COCC1>[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([CH2:29][NH:1][C:2]3[CH:15]=[CH:14][C:5]([CH2:6][N:7]4[C:11](=[O:12])[N-:10][C:9](=[O:13])[O:8]4)=[CH:4][CH:3]=3)[CH:24]=2)=[C:19]([CH3:31])[CH:18]=1.[Na+:49]
参加物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 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 18624553HCID 18624553、化合物HCID 86632832HCID 86632832、化合物

生成物 1

HCID 57787267HCID 57787267、化合物収率 14.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-(4-aminobenzyl)-1,2,4-oxadiazolidine-3,5-dione (500 mg), 4′-chloro-2′-methylbiphenyl-3-carbaldehyde (668 mg), acetic acid (0.33 ml) and THF (40 ml) was stirred at room temperature for 24 hours. Sodium triacetoxyborohydride (767 mg) was added to the reaction mixture, followed by stirring at room temperature for 15 minutes. The solvent was evaporated under a reduced pressure, and water was added to the residue, followed by extraction with chloroform. The organic layer was washed with a saturated sodium chloride aqueous solution, the solvent was evaporated under a reduced pressure, toluene was added to the residue, and the solvent was again evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate), and THF (5 ml), methanol (5 ml) and a 1 M sodium hydroxide aqueous solution (1.47 ml) were added to the resulting pale yellow foamy substance (620 mg), followed by stirring at room temperature for 5 minutes. The solvent was evaporated under a reduced pressure, the residue was purified by an ODS column chromatography (water-acetonitrile) and made into a solid by adding diethyl ether. The solid was collected by filtration and then dried by heating under a reduced pressure to obtain sodium 2-(4-{[(4′-chloro-2′-methylbiphenyl-3-yl)methyl]amino}benzyl)3,5-dioxo-1,2,4-oxadiazolidin-4-ide (160 mg) as a white solid.

後処理

  1. stirringby stirring at room temperature for 15 minutes
  2. customThe solvent was evaporated under a reduced pressure, and water
  3. additionwas added to the residue
  4. extractionfollowed by extraction with chloroform
  5. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  6. customthe solvent was evaporated under a reduced pressure, toluene
  7. additionwas added to the residue
  8. customthe solvent was again evaporated under a reduced pressure
  9. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate), and THF (5 ml), methanol (5 ml)
  10. additiona 1 M sodium hydroxide aqueous solution (1.47 ml) were added to the resulting pale yellow foamy substance (620 mg)
  11. stirringby stirring at room temperature for 5 minutes
  12. customThe solvent was evaporated under a reduced pressure
  13. customthe residue was purified by an ODS column chromatography (water-acetonitrile)
  14. additionby adding diethyl ether
  15. filtrationThe solid was collected by filtration
  16. customdried
  17. temperatureby heating under a reduced pressure

出典と根拠

ORDレコード
ord-0946fa90aa494d8bb1395948e2aa8310
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07968552B2

反応ノート

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