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

Aniline → N-[[[4-(6-bromo-1,3-benzodioxan-2-yl)phenyl]amino]carbonyl]-2,6,-difluorobenzamide

HRID 1708176
ノート
印刷プレビュー

反応式

HRID 1708176 の反応式
[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][CH:7]([C:10]3[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][CH:11]=3)[O:8][CH2:9][C:4]=2[CH:3]=1.[H][H].C(=O)([O-])[O-].[K+].[K+].NC1C=CC=CC=1.[F:36][C:37]1[CH:47]=[CH:46][CH:45]=[C:44]([F:48])[C:38]=1[C:39]([N:41]=[C:42]=[O:43])=[O:40]>C1(C)C=CC=CC=1.[Pt]>[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][CH:7]([C:10]3[CH:15]=[CH:14][C:13]([NH:16][C:42]([NH:41][C:39](=[O:40])[C:38]4[C:44]([F:48])=[CH:45][CH:46]=[CH:47][C:37]=4[F:36])=[O:43])=[CH:12][CH:11]=3)[O:8][CH2:9][C:4]=2[CH:3]=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

8

反応物 5

HCID 6115AnilineHCID 11430Potassium CarbonateHCID 27333692,6-Difluorobenzoyl isocyanateHCID 189611956-Bromo-2-(4-nitrophenyl)-1,3-benzodioxanHCID 178418361HCID 178418361、化合物

生成物 1

HCID 18961193N-[[[4-(6-bromo-1,3-benzodioxan-2-yl)phenyl]amino]carbonyl]-2,6,-difluorobenzamide

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 1140Toluene溶媒2 回

反応条件

温度
60 °C

実験手順

A suspension of 6-bromo-2-(4-nitrophenyl)-1,3-benzodioxan (2.05 g) in toluene (150 ml) was hydrogenated at ≤60 psi hydrogen pressure in the presence of 5% platinum/charcoal (0.5 g) and anhydrous potassium carbonate (0.5 g) at ambient temperature. The reaction mixture was filtered and evaporated under reduced pressure, azeotropically removing the water formed in the reaction. The resulting crude aniline derivative was redissolved in dry toluene (25 ml) and treated with 2,6-difluorobenzoyl isocyanate (1.2 g), warming briefly to approx. 60° C. then allowing the stirred reaction mixture to cool overnight. Cooling to 0°-5° C. afforded a precipitate of impure product which was purified by crystallisation from ethanol (0.52 g, 17%), mp 194°-195° C.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customevaporated under reduced pressure
  3. customazeotropically removing the water
  4. customformed in the reaction
  5. customthe stirred reaction mixture
  6. temperatureto cool overnight
  7. temperatureCooling to 0°-5° C.
  8. customafforded a precipitate of impure product which
  9. customwas purified by crystallisation from ethanol (0.52 g, 17%), mp 194°-195° C.

出典と根拠

ORDレコード
ord-c76d30b020a842a4b830bb5e106f322f
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05356924

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