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

Methyl iodide → HCID 18674213、化合物

HRID 1635929
ノート
印刷プレビュー

反応式

HRID 1635929 の反応式
[H-].[Na+].[NH2:3][C:4]1[C:8]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[C:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[NH:6][N:5]=1.[CH3:22]I>CN(C)C=O>[NH2:3][C:4]1[C:8]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[C:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[N:6]([CH3:22])[N:5]=1.[NH2:3][C:4]1[N:5]([CH3:22])[N:6]=[C:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:8]=1[C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=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 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 155131013-Amino-5-(4-fluorophenyl)-4-(4-pyridyl)pyrazole

生成物 2

HCID 18674082HCID 18674082、化合物収率 32%HCID 18674213HCID 18674213、化合物収率 43%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
3 回

実験手順

While a dimethylformamide suspension containing 0.17 g of 60% sodium hydride was being cooled with ice, 10 ml of a dimethylformamide solution containing 1.00 g of 3-amino-5-(4-fluorophenyl)-4-(4-pyridyl)pyrazole was added dropwise thereto, followed by stirring at room temperature for 30 minutes. Then, 5 ml of a dimethylformamide solution containing 0.67 g of methyl iodide was added dropwise thereto, followed by stirring at room temperature for 3 hours. After the dimethylformamide was distilled off under reduced pressure, the resulting residue was extracted with chloroform. The organic layer was washed with water and dried over anhydrous magnesium sulfate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by column chromatography using 250 g of silica gel [with an elution solvent comprising chloroform-methanol (20:1)]. Thus, 0.34 g (32% yield) of 3-amino-5-(4-fluorophenyl)-1-methyl-4-(4-pyridyl)pyrazole (light-brown crystals) was obtained as a first elution product, and 0.45 g (43% yield) of 5-amino-3-(4-fluorophenyl)-1-methyl-4-(4-pyridyl)pyrazole (light-brown crystals) as a second elution product.

後処理

  1. additionwas added dropwise
  2. additionwas added dropwise
  3. stirringby stirring at room temperature for 3 hours
  4. distillationAfter the dimethylformamide was distilled off under reduced pressure
  5. extractionthe resulting residue was extracted with chloroform
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationAfter the solvent was distilled off under reduced pressure
  9. customthe resulting residue was purified by column chromatography

出典と根拠

ORDレコード
ord-725aec7adf2f4e578161b39580c0be56
出典データセット
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06511997B1

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