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Hydroxylamine HCl → 3-[2-(4-ethoxyphenyl)-2-oxoethyl]-6-ethyl-1-{[2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

HRID 1889496
ノート
印刷プレビュー

反応式

HRID 1889496 の反応式
[CH2:1]([C:3]1[S:28][C:6]2[N:7]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20]4[C:21]([C:26]#[N:27])=[CH:22][CH:23]=[CH:24][CH:25]=4)=[CH:16][CH:15]=3)[C:8](=[O:12])[NH:9][C:10](=[O:11])[C:5]=2[CH:4]=1)[CH3:2].Br[CH2:30][C:31]([C:33]1[CH:38]=[CH:37][C:36]([O:39][CH2:40][CH3:41])=[CH:35][CH:34]=1)=[O:32].[H-].[Na+].[Cl-].O[NH3+:46].[C:47](=[O:50])([O-])[OH:48].[Na+]>C(OCC)(=O)C.CS(C)=O.C(Cl)(Cl)Cl.CN(C)C=O>[CH2:40]([O:39][C:36]1[CH:37]=[CH:38][C:33]([C:31](=[O:32])[CH2:30][N:9]2[C:10](=[O:11])[C:5]3[CH:4]=[C:3]([CH2:1][CH3:2])[S:28][C:6]=3[N:7]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]4[NH:46][C:47](=[O:50])[O:48][N:27]=4)=[CH:16][CH:15]=3)[C:8]2=[O:12])=[CH:34][CH:35]=1)[CH3:41]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 21645Hydroxylamine HClHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 21130602-Bromo-1-(4-ethoxyphenyl)ethanoneHCID 593517704'-[(6-ethyl-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl)methyl]biphenyl-2-carbonitrile

生成物 1

HCID 136052256
3-[2-(4-ethoxyphenyl)-2-oxoethyl]-6-ethyl-1-{[2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione
収率 16.1%

試薬・触媒・溶媒 4

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of 4′-[(6-ethyl-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl)methyl]biphenyl-2-carbonitrile (1.5 g), 2-bromo-1-(4-ethoxyphenyl)ethanone (1.14 g) and N,N-dimethylformamide (30 mL) was added sodium hydride (0.19 g), and the mixture was stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate, washed successively with 5% aqueous potassium hydrogensulfate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue obtained by silica gel column chromatography was dissolved in dimethyl sulfoxide (5 mL), and the mixture was added to a mixture of hydroxylammonium chloride (1 g), sodium hydrogencarbonate (1.15 g) and dimethyl sulfoxide (10 mL), which had been stirred at 40° C. for 30 min in advance. The reaction mixture was stirred at 90° C. for 16 hr, diluted with chloroform, washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography and dissolved in methylene chloride (20 mL). N,N′-Carbonyldiimidazole (0.3 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.25 mL) were added, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with chloroform, washed successively with saturated aqueous potassium hydrogensulfate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by preparative HPLC to give the title compound as colorless crystals (0.38 g, 16%).

後処理

  1. washwashed successively with 5% aqueous potassium hydrogensulfate solution and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue obtained by silica gel column chromatography
  5. stirringhad been stirred at 40° C. for 30 min in advance
  6. stirringThe reaction mixture was stirred at 90° C. for 16 hr
  7. washwashed successively with water and saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. customThe residue was purified by silica gel column chromatography
  11. dissolutiondissolved in methylene chloride (20 mL)
  12. additionN,N′-Carbonyldiimidazole (0.3 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.25 mL) were added
  13. stirringthe mixture was stirred at room temperature for 2 hr
  14. additionThe reaction mixture was diluted with chloroform
  15. washwashed successively with saturated aqueous potassium hydrogensulfate solution and saturated brine
  16. dry with materialdried over anhydrous magnesium sulfate
  17. customThe solvent was evaporated under reduced pressure
  18. customThe obtained residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-c30ce60f048445beab2e0727c1ec6cb0
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501750B2

反応ノート

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