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

4-tert-Butylbenzenesulfonamide → HCID 22282042、化合物

HRID 1368632
ノート
印刷プレビュー

反応式

HRID 1368632 の反応式
[CH3:1][O:2][C:3]1[C:7]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH3:16])=[C:6]([NH2:17])[N:5]([CH3:18])[N:4]=1.[C:19]([C:23]1[CH:28]=[CH:27][C:26]([S:29](N)(=[O:31])=[O:30])=[CH:25][CH:24]=1)([CH3:22])([CH3:21])[CH3:20]>CN(C)C1C=CN=CC=1.N1C=CC=CC=1.C(O)C.[OH-].[Na+].Cl>[C:19]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH:17][C:6]2[N:5]([CH3:18])[N:4]=[C:3]([O:2][CH3:1])[C:7]=2[O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH3:16])(=[O:31])=[O:30])=[CH:25][CH:24]=1)([CH3:22])([CH3:20])[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 2

HCID 2228724-tert-Butylbenzenesulfonamide2 回HCID 22281998HCID 22281998、化合物

生成物 1

HCID 22282042HCID 22282042、化合物収率 33.6%

試薬・触媒・溶媒 5

HCID 142844-(Dimethylamino)pyridine触媒HCID 313Hydrochloric Acid溶媒HCID 702Ethanol
溶媒
HCID 1049Pyridine溶媒
HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 3-methoxy-4-(2-methoxyphenoxy)-1-methyl-1H-pyrazol-5-amine (Preparation 68) (45 mg), (4-tert-butyl)benzenesulfonamide (42 mg) and 4-dimethylaminopyridine (22 mg) in dry pyridine (2 ml) was stirred at room temperature for 16 hours. A further aliquot of (4-tert-butyl)benzenesulfonamide (42 mg) was added to the reaction mixture and stirring at room temperature was continued for a further 24 hours. The reaction mixture was diluted with ethanol (2 ml) and 1.0M aqueous sodium hydroxide solution (4 ml) and was then stirred at room temperature for 4 hours. The mixture was diluted with aqueous 1.0M hydrochloric acid (20 ml) and then extracted with ethyl acetate (3×15 ml). The combined organic extracts were washed with aqueous 1.0M hydrochloric acid (20 ml), dried (magnesium sulfate) and then concentrated under vacuum. The residue was purified by chromatography on silica (5 g) using 40% ethyl acetate/pentane as eluant to give the title compound as an off-white solid (27 mg), Rf 0.85 (ethyl acetate), m.p. 187.6° C.

後処理

  1. stirringwas then stirred at room temperature for 4 hours
  2. extractionextracted with ethyl acetate (3×15 ml)
  3. washThe combined organic extracts were washed with aqueous 1.0M hydrochloric acid (20 ml)
  4. dry with materialdried (magnesium sulfate)
  5. concentrationconcentrated under vacuum
  6. customThe residue was purified by chromatography on silica (5 g)

出典と根拠

ORDレコード
ord-dcb053b6797a49d58799a8ec6cab2d7b
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06573270B1

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