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 Dithionite → n-{3-Amino-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

HRID 840096
ノート
印刷プレビュー

反応式

HRID 840096 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([NH:26][S:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)(=[O:29])=[O:28])[CH:7]=[CH:8][C:9]=1[NH:10][CH2:11][C:12]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[C:14]([C:22]([F:25])([F:24])[F:23])[CH:13]=1)([O-])=O.[O-]S(S([O-])=O)=O.[Na+].[Na+]>CO.O>[NH2:1][C:4]1[CH:5]=[C:6]([NH:26][S:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)(=[O:28])=[O:29])[CH:7]=[CH:8][C:9]=1[NH:10][CH2:11][C:12]1[CH:17]=[C:16]([C:18]([F:21])([F:19])[F:20])[CH:15]=[C:14]([C:22]([F:23])([F:24])[F:25])[CH:13]=1
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 2

HCID 24489Sodium DithioniteHCID 22621842n-{3-Nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

生成物 1

HCID 22621789n-{3-Amino-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

N-{3-nitro-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide (8.6 g, 16.6 mmol) in 200 mL methanol are refluxed and within 0.5 h combined with a solution of Na2S2O4 (14.2 g, mmol) in 50 mL water. The mixture is refluxed until totally decolorised (this takes about 1 h). After cooling the mixture is diluted with water. About 100 mL of the methanol/water mixture are distilled off, the resulting solution is cooled, the crystals precipitated are filtered off and washed with water. The crystals are dissolved in ethyl acetate, dried and evaporated down until not quite dry. After cooling the crystals precipitated are filtered off and washed with diethylether.

後処理

  1. temperatureThe mixture is refluxed
  2. customthis takes about 1 h
  3. temperatureAfter cooling the mixture
  4. distillationAbout 100 mL of the methanol/water mixture are distilled off
  5. temperaturethe resulting solution is cooled
  6. customthe crystals precipitated
  7. filtrationare filtered off
  8. washwashed with water
  9. dissolutionThe crystals are dissolved in ethyl acetate
  10. customdried
  11. customevaporated down until not
  12. customquite dry
  13. temperatureAfter cooling the crystals
  14. customprecipitated
  15. filtrationare filtered off
  16. washwashed with diethylether

出典と根拠

ORDレコード
ord-333675e0e8684ec5bd7421fcf0cac065
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06365584B1

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