ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Water → (E)-(6S,8S,9aR)-8-fluoro-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]-6-(3,4,5-trifluorophenyl)octahydroquinolizin-4-one

HRID 553947
ノート
印刷プレビュー

反応式

HRID 553947 の反応式
C(N(S(F)(F)[F:7])CC)C.[F:10][C:11]1[CH:12]=[C:13]([C@@H:19]2[CH2:28][C@H:27](O)[CH2:26][C@@H:25]3[N:20]2[C:21](=[O:45])/[C:22](=[CH:30]/[C:31]2[CH:36]=[CH:35][C:34]([N:37]4[CH:41]=[C:40]([CH3:42])[N:39]=[CH:38]4)=[C:33]([O:43][CH3:44])[CH:32]=2)/[CH2:23][CH2:24]3)[CH:14]=[C:15]([F:18])[C:16]=1[F:17].O.C(OCC)(=O)C>ClCCl>[F:7][C@H:27]1[CH2:26][C@@H:25]2[N:20]([C:21](=[O:45])/[C:22](=[CH:30]/[C:31]3[CH:36]=[CH:35][C:34]([N:37]4[CH:41]=[C:40]([CH3:42])[N:39]=[CH:38]4)=[C:33]([O:43][CH3:44])[CH:32]=3)/[CH2:23][CH2:24]2)[C@H:19]([C:13]2[CH:14]=[C:15]([F:18])[C:16]([F:17])=[C:11]([F:10])[CH:12]=2)[CH2:28]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 962WaterHCID 8857Ethyl AcetateHCID 123472(Diethylamino)sulfur trifluorideHCID 24781747(E)-(6S*,8R*,9aR*)-6-(3,4,5-trifluorophenyl)-8-hydroxy-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]octahydroquinolizin-4-one

生成物 1

HCID 24780877(E)-(6S,8S,9aR)-8-fluoro-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]-6-(3,4,5-trifluorophenyl)octahydroquinolizin-4-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Diethylaminosulfur trifluoride (13.2 μL) was added to a solution of (E)-(6S,8R,9aR)-6-(3,4,5-trifluorophenyl)-8-hydroxy-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]octahydroquinolizin-4-one that is an optically active compound obtained above with a retention time of 4.8 minutes (10 mg) in dichloromethane (2.0 mL) under ice-cooling, and the reaction solution was stirred for two hours. Crushed ice, water, and ethyl acetate were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system->ethyl acetate-methanol system) to obtain 5.9 mg of the title optically active compound. The property values of the optically active compound are as follows.

後処理

  1. temperaturecooling
  2. customthe organic layer was separated
  3. washThe resulting organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system->ethyl acetate-methanol system)
  7. customto obtain 5.9 mg of the title optically active compound

出典と根拠

ORDレコード
ord-6ca660ae38aa4007ba21e6b5ce977209
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08048878B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート