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

Pyridine → Pyrazosulfuron-ethyl

HRID 260139
ノート
印刷プレビュー

反応式

HRID 260139 の反応式
[O-:1][C:2]#[N:3].[Na+].[NH2:5][C:6]1[N:11]=[C:10]([O:12][CH3:13])[CH:9]=[C:8]([O:14][CH3:15])[N:7]=1.N1C=CC=CC=1.[CH3:22][N:23]1[C:27]([S:28](Cl)(=[O:30])=[O:29])=[C:26]([C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:25]=[N:24]1>C(#N)C>[CH3:13][O:12][C:10]1[CH:9]=[C:8]([O:14][CH3:15])[N:7]=[C:6]([NH:5][C:2]([NH:3][S:28]([C:27]2[N:23]([CH3:22])[N:24]=[CH:25][C:26]=2[C:32]([O:34][CH2:35][CH3:36])=[O:33])(=[O:30])=[O:29])=[O:1])[N:11]=1
参加物反応条件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 1049PyridineHCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 517096Sodium CyanateHCID 10977963ethyl 5-(chlorosulfonyl)-1-methyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 91750Pyrazosulfuron-ethyl収率 98%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

反応条件

温度
45 °C

実験手順

7.27 g of anhydrous sodium cyanate, 15.78 g of 2-amino-4,6-dimethoxypyrimidine, 8.04 g of pyridine and 40 g of dry acetonitrile were mixed together and the mixture was warmed to 45° C. under nitrogen atmosphere. To this mixture was added 28.46 g of 1-methyl-4-ethoxycarbonylpyrazole-5-sulfonylchloride over 2 hours and the reaction mixture was stirred for further 2 hours while maintaining the temperature of 45° C. After the completion of the reaction was identified by liquid chromatography, the reaction product was extracted with 200 g of dichloromethane and 40 g of 5% aqueous sulfuric acid solution. The extracted organic layer was dried over anhydrous magnesium sulfate and then filtered. The organic solvent was removed from the product to obtain 41.30 g (Yield 98%) of the title compound as a solid state.

後処理

  1. temperaturewhile maintaining the temperature of 45° C
  2. extractionthe reaction product was extracted with 200 g of dichloromethane and 40 g of 5% aqueous sulfuric acid solution
  3. dry with materialThe extracted organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe organic solvent was removed from the product

出典と根拠

ORDレコード
ord-e584c653c3d843989d44858f8ab76e70
出典データセット
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05525730

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート