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

Dimethyl Sulfide → 6-(6-Bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2h)-pyridazinone

HRID 915051
ノート
印刷プレビュー

反応式

HRID 915051 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[N:18]=[C:17]([C:19]2[CH:20]=[CH:21][C:22](=[O:28])[N:23]([CH:25]([CH3:27])[CH3:26])[N:24]=2)[C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:15][C:14]=1[N:35]=S(C)C.CSC.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[Br:12][C:13]1[N:18]=[C:17]([C:19]2[CH:20]=[CH:21][C:22](=[O:28])[N:23]([CH:25]([CH3:27])[CH3:26])[N:24]=2)[C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:15][C:14]=1[N:35]=[O:9]
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 1068Dimethyl SulfideHCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 877986596-{6-bromo-5-[(dimethyl-lambda~4~-sulfanylidene)amino]-3-phenyl-2-pyrazinyl}-2-isopropyl-3 (2H)-pyridazinone

生成物 1

HCID 877873306-(6-Bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2h)-pyridazinone収率 49.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of m-chloroperbenzoic acid (70-75% purity) (1.66 g) in CH2Cl2 (40 ml) was added a solution of 6-{6-bromo-5-[(dimethyl-lambda˜4˜-sulfanylidene)amino]-3-phenyl-2-pyrazinyl}-2-isopropyl-3 (2H)-pyridazinone (2.01 g) in CH2Cl2 (20 ml) at −10˜-5° C. and the mixture was stirred at the same temperature for one hour. After addition of dimethyl sulfide (0.25 ml), the solution was stirred at the same temperature for 30 minutes. Sat. aq. Na2CO3 (50 ml) was then added to the mixture. An organic layer was collected, dried over MgSO4, concentrated under reduced pressure and purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (70:30 v/v) to give 6-(6-bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone as a solid (0.896 g).

後処理

  1. stirringthe solution was stirred at the same temperature for 30 minutes
  2. customAn organic layer was collected
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. custompurified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (70:30 v/v)

出典と根拠

ORDレコード
ord-d1997d09c60b4596949a9a39b9828b96
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265120B2

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