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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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Dichloromethane → Rivaroxaban

HRID 1054153
ノート
印刷プレビュー

反応式

HRID 1054153 の反応式
[O:1]=[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][C:14]3=[O:19])=[CH:9][CH:8]=2)[CH2:5][C@H:4]([CH2:20][NH:21][CH:22]=[O:23])[O:3]1.ClCCl.[N+](C1C=CC([C:36]2[CH:40]=[C:39]([Cl:41])[S:38][C:37]=2C([O-])=O)=CC=1)([O-])=O.[OH-].[Na+]>O.CO.C(O)(=O)C>[CH:11]1[C:10]([N:13]2[C:14](=[O:19])[CH2:15][O:16][CH2:17][CH2:18]2)=[CH:9][CH:8]=[C:7]([N:6]2[C:2](=[O:1])[O:3][C@@H:4]([CH2:20][NH:21][C:22]([C:37]3[S:38][C:39]([Cl:41])=[CH:40][CH:36]=3)=[O:23])[CH2:5]2)[CH:12]=1
参加物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 6344Dichloromethane2 回HCID 14798Sodium HydroxideHCID 90258317Rivaroxaban Impurity 116HCID 902586624-Nitrophenyl-5-chlorothiophene-2-carboxylate

生成物 1

HCID 9875401Rivaroxaban

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒
HCID 887
Methanol
溶媒
HCID 962Water溶媒

実験手順

N-({(5 S)-2-oxo-3-[4-(3-oxomorpholin-4-yl)phenyl]-1,3-oxazolidin-5-yl}methyl)formamide (1 g) taken in a dichloromethane(10 ml) and stirred reaction mass at 25 to 30° C. for 30 minutes. To this mixture added solution of 4-nitrophenyl-5-chlorothiophene-2-carboxylate (1.06 g) in a dichloromethane (10 ml) and sodium hydroxide (0.38 g) in water (5 ml) simultaneously through addition funnel. Obtained reaction mass then stirred for 1 to 2 h at 25 to 30° C. After completion of reaction, Separated organic layer and concentrated under reduced pressure to obtain residue. Added acetic acid and methanol to residue stirred for 30 minutes and obtained solid is filtered off. Washed solid with methanol.

後処理

  1. customreaction mass at 25 to 30° C. for 30 minutes
  2. additionsimultaneously through addition funnel
  3. customObtained
  4. customreaction mass
  5. stirringthen stirred for 1 to 2 h at 25 to 30° C
  6. customAfter completion of reaction
  7. customSeparated organic layer
  8. concentrationconcentrated under reduced pressure
  9. customto obtain residue
  10. customobtained solid
  11. filtrationis filtered off
  12. washWashed solid with methanol

出典と根拠

ORDレコード
ord-ecaac78c675f493183d48d548706c34e
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394292B2

反応ノート

読み込み中…

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