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Hydroxyamine hydrochloride → tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-{[2-oxo-3-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)pyridin-1(2H)-yl]methyl}-1,4-oxazepane-4-carboxylate

HRID 1022605
ノート
印刷プレビュー

反応式

HRID 1022605 の反応式
[C:1](=[O:4])([O-])[OH:2].[Na+].Cl.NO.[C:9]([C:11]1[C:12](=[O:40])[N:13]([CH2:17][C@H:18]2[C@H:24]([C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([Cl:32])[CH:26]=3)[O:23][CH2:22][CH2:21][N:20]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[CH2:19]2)[CH:14]=[CH:15][CH:16]=1)#[N:10].C1(C2CCCCCCCCCC=2)CCCCCCCCN[N:42]=1>CS(C)=O.O.C1COCC1>[Cl:32][C:27]1[CH:26]=[C:25]([C@@H:24]2[O:23][CH2:22][CH2:21][N:20]([C:33]([O:35][C:36]([CH3:37])([CH3:39])[CH3:38])=[O:34])[CH2:19][C@H:18]2[CH2:17][N:13]2[CH:14]=[CH:15][CH:16]=[C:11]([C:9]3[NH:42][C:1](=[O:4])[O:2][N:10]=3)[C:12]2=[O:40])[CH:30]=[CH:29][C:28]=1[Cl:31]
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

8

反応物 4

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 536302743-(Cycloundecen-1-yl)-1,2-diazacycloundec-2-eneHCID 66975537tert-butyl (6R,7R)-6-[(3-cyano-2-oxopyridin-1(2H)-yl)methyl]-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

生成物 1

HCID 136340695
tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-{[2-oxo-3-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)pyridin-1(2H)-yl]methyl}-1,4-oxazepane-4-carboxylate
収率 72.6%

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

Sodium hydrogen carbonate (829 mg, 9.87 mmol) and hydroxylamine hydrochloride (686 mg, 9.87 mmol) were added to a solution of tert-butyl (6R,7R)-6-[(3-cyano-2-oxopyridin-1(2H)-yl)methyl]-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (590 mg, 1.23 mmol) in DMSO (4 mL), and the mixture was stirred at 80° C. for 5 hr. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was diluted with THF (10 mL), diazabicycloundecene (0.184 mL, 1.23 mmol) and carbonyl-1,1′-bisimidazole (299 mg, 1.85 mmol) were added, and the mixture was stirred at 70° C. for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was acidified with 1 N hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography, and recrystallized from ethanol-hexane to give the title compound (480 mg, 0.893 mmol, 72.6%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. additionwere added
  6. stirringthe mixture was stirred at 70° C. for 2 hr
  7. concentrationThe reaction mixture was concentrated under reduced pressure
  8. extractionthe mixture was extracted with ethyl acetate
  9. washThe extract was washed with brine
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was evaporated under reduced pressure
  12. customThe residue was purified by silica gel column chromatography
  13. customrecrystallized from ethanol-hexane

出典と根拠

ORDレコード
ord-a66d52cb102048e0b228a4c272522d6e
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

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