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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Nitric Acid → [(4aR,6R,8aS)-2-amino-8a-(2-fluoro-5-nitrophenyl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-6-yl]methanol

HRID 217992
ノート
印刷プレビュー

反応式

HRID 217992 の反応式
S(=O)(=O)(O)O.[NH2:6][C:7]1[S:16][CH2:15][C@H:14]2[C@:9]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[F:25])([CH2:10][O:11][C@@H:12]([CH2:17][OH:18])[CH2:13]2)[N:8]=1.[N+:26]([O-])([OH:28])=[O:27].[OH-].[Na+]>C(O)(C(F)(F)F)=O>[NH2:6][C:7]1[S:16][CH2:15][C@H:14]2[C@:9]([C:19]3[CH:24]=[C:23]([N+:26]([O-:28])=[O:27])[CH:22]=[CH:21][C:20]=3[F:25])([CH2:10][O:11][C@@H:12]([CH2:17][OH:18])[CH2:13]2)[N:8]=1
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 944Nitric AcidHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 58406040[(4aR,6R,8aS)-2-amino-8a-(2-fluorophenyl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-6-yl]methanol

生成物 1

HCID 58406109[(4aR,6R,8aS)-2-amino-8a-(2-fluoro-5-nitrophenyl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-6-yl]methanol

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

Concentrated sulfuric acid (2.5 ml) was added dropwise to a solution of [(4aR,6R,8aS)-2-amino-8a-(2-fluorophenyl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-6-yl]methanol (700 mg) in TFA (5 ml) in an ice bath. Then, fuming nitric acid (specific gravity: 1.52, 103 μl) was added dropwise at the same temperature, followed by stirring for one hour. The reaction mixture was poured into ice and made basic with a 5 N sodium hydroxide solution, followed by stirring at room temperature for two hours. The aqueous layer was extracted with dichloromethane, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to obtain the title compound (1.0 g).

後処理

  1. additionThe reaction mixture was poured into ice
  2. stirringby stirring at room temperature for two hours
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-51bd7574f6784e3795a2d39b89ce72a5
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08198269B2

反応ノート

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