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

Dimethylacetamide → HCID 59129370、化合物

HRID 1847818
ノート
印刷プレビュー

反応式

HRID 1847818 の反応式
[C:1]([C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][C:6]=1[N+:15]([O-:17])=[O:16])([CH3:4])([CH3:3])[CH3:2].C(C1C=CC([N+]([O-])=O)=C(C)C=1[N+]([O-])=O)(C)(C)C.C[C:36]([N:38]([CH3:40])[CH3:39])=O>CN(C=O)C>[C:1]([C:5]1[C:6]([N+:15]([O-:17])=[O:16])=[CH:7][C:8]([N+:12]([O-:14])=[O:13])=[C:9](/[CH:11]=[CH:36]/[N:38]([CH3:40])[CH3:39])[CH:10]=1)([CH3:4])([CH3:2])[CH3:3]
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 31374DimethylacetamideHCID 533645731-Tert-butyl-5-methyl-2,4-dinitrobenzeneHCID 591294471-Tert-butyl-3-methyl-2,4-dinitrobenzene

生成物 1

HCID 59129370HCID 59129370、化合物収率 68%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-tert-butyl-5-methyl-2,4-dinitrobenzene and 1-tert-butyl-3-methyl-2,4-dinitrobenzene (9.0 g, 38 mmol, 2:1 by NMR) and DMA (5.4 g, 45 mmol) in DMF (50 mL) was heated at reflux for 2 h before being cooled to room temperature. The reaction mixture was poured into water-ice and extracted with EtOAc (50 mL×3). The combined organic layers were washed with water and brine, before being evaporated to give a brown oil, which was purified by column to give (E)-2-(5-tert-butyl-2,4-dinitrophenyl)-N,N-dimethylethen-amine (5.0 g, 68%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. extractionextracted with EtOAc (50 mL×3)
  4. washThe combined organic layers were washed with water and brine
  5. custombefore being evaporated
  6. customto give a brown oil, which
  7. customwas purified by column

出典と根拠

ORDレコード
ord-2f16bc5509964fd78078af437e473b26
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952049B2

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