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

Sodium Bicarbonate → 2-(2-chlorobenzyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one

HRID 1455244
ノート
印刷プレビュー

反応式

HRID 1455244 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH2:4][C:5]1[C:12](=[O:13])[N:8]2[CH2:9][CH2:10][CH2:11][N:7]2[C:6]=1[C:14]1[CH:19]=[CH:18][N:17]=[C:16](SC)[N:15]=1.O[O:27][S:28]([O-:30])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+].[C:40]([O-])(O)=O.[Na+]>C1COCC1.CO.O>[Cl:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH2:4][C:5]1[C:12](=[O:13])[N:8]2[CH2:9][CH2:10][CH2:11][N:7]2[C:6]=1[C:14]1[CH:19]=[CH:18][N:17]=[C:16]([S:28]([CH3:40])(=[O:30])=[O:27])[N:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 516892Sodium BicarbonateHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 574380712-(2-chlorobenzyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one

生成物 1

HCID 574380742-(2-chlorobenzyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To a cold 0° C. solution of 2-(2-chlorobenzyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one, 7, (460 mg, 1.23 mmol)) in THF/MeOH (20 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (3.0 g, 4.9 mmol) in H2O (15 mL). After stirring the reaction for 1.5 hours at room temperature, the solution is poured into aqueous saturated NaHCO3. The aqueous phase is extracted three times with EtOAc and the combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated in vacuo to afford 316 mg of the desired product which is used without further purification.

後処理

  1. customthe reaction for 1.5 hours at room temperature
  2. extractionThe aqueous phase is extracted three times with EtOAc
  3. washthe combined organic layers are washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1f2185a3519e49a3944fd90d5a7c7b7b
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482356B2

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