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 Hydroxide → 4-(Butane-1-sulfonyl)-1-methyl-3,5-diphenyl-1H-pyrazole

HRID 441531
ノート
印刷プレビュー

反応式

HRID 441531 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:16][C:17]1[C:18]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:19][N:20]([CH3:28])[C:21]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH2:13][CH2:14][CH3:15].[OH-:35].[Na+]>C(Cl)(Cl)Cl>[CH2:12]([S:16]([C:17]1[C:18]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:19][N:20]([CH3:28])[C:21]=1[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)(=[O:9])=[O:35])[CH2:13][CH2:14][CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 213980704-(Butylsulfanyl)-1-methyl-3,5-diphenyl-1H-pyrazole

生成物 1

HCID 213981084-(Butane-1-sulfonyl)-1-methyl-3,5-diphenyl-1H-pyrazole収率 61%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of m-chloroperbenzoic acid (10.15 g, 85%, 0.05 mole) in dry chloroform (100 ml) is added to 4-(n-butylthio)-1-methyl-3,5-diphenylpyrazole (6.5 g, 0.02 mole) in dry chloroform (50 ml) and the reaction mixture stirred overnight at 10° C. to 12° C. The mixture is poured into 10% aqueous sodium hydroxide (200 ml) and extracted with chloroform. The chloroform layer is separated, dried and stripped in vacuo to give a light-orange oil. The oil is chromatographed on silca gel with benzene. The fractions containing the product are combined, stripped in vacuo, extracted with methanol, filtered, stripped in vacuo and then recrystallized from hexane to give a white fluffy solid 4.37 g (61%), m.p. 92.5° C. to 93° C.

後処理

  1. extractionextracted with chloroform
  2. customThe chloroform layer is separated
  3. customdried
  4. customto give a light-orange oil
  5. customThe oil is chromatographed on silca gel with benzene
  6. additionThe fractions containing the product
  7. extractionextracted with methanol
  8. filtrationfiltered
  9. customrecrystallized from hexane

出典と根拠

ORDレコード
ord-7a5d268d382040399a72c646745b8268
出典データセット
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04041046

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