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

Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → ethyl (2Z)-3-[(4-bromo-3-methoxyphenyl)amino]-3-phenylacrylate

HRID 1360103
ノート
印刷プレビュー

反応式

HRID 1360103 の反応式
[CH3:1][NH:2]/[C:3](/[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[CH:4]\[C:5]([O:7][CH2:8][CH3:9])=[O:6].[Br:16][C:17]1[CH:23]=[CH:22]C(N)=[CH:19][C:18]=1[O:24][CH3:25].CC1C=CC(S([O-])(=O)=O)=CC=1.C1C=C[NH+]=CC=1>C(Cl)Cl>[Br:16][C:17]1[CH:23]=[CH:22][C:1]([NH:2]/[C:3](/[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:4]\[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:19][C:18]=1[O:24][CH3:25]
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 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 70182544-Bromo-3-methoxyanilineHCID 10976613ethyl (2Z)-3-(methylamino)-3-phenylacrylate

生成物 1

HCID 57617098ethyl (2Z)-3-[(4-bromo-3-methoxyphenyl)amino]-3-phenylacrylate収率 87.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of ethyl (2Z)-3-(methylamino)-3-phenylacrylate (4.47 g, 21.77 mmol) in DCM (100 mL) was added 4-bromo-3-methoxyaniline (4 g, 19.80 mmol) and PPTS (5.47 g, 21.77 mmol). The mixture was then heated to reflux for 24 h. At this time crude 1H NMR revealed nearly complete consumption of the aniline. The reaction was then cooled to RT, filtered, and the solvent was removed in vacuo. The crude product was purified on silica (75% DCM/hexanes) to yield ethyl (2Z)-3-[(4-bromo-3-methoxyphenyl)amino]-3-phenylacrylate (6.5 g, 87%) which was used as is in subsequent reactions. 1H NMR (500 MHz, CDCl3) ppm: 10.32 (br s, 1H), 7.32 (m, 5H), 7.20 (d, J=8.5 Hz, 1H), 6.19 (dd, J=8.5 Hz, 2.5 Hz, 1H), 6.11 (d, J=2.5 z, 1H), 5.03 (s, 1H), 4.21 (q, J=7.0 Hz, 2H), 3.50 (s, 3H), 1.32 (t, J=7.0 Hz, 3H).

後処理

  1. temperatureThe mixture was then heated
  2. temperatureto reflux for 24 h
  3. customconsumption of the aniline
  4. filtrationfiltered
  5. customthe solvent was removed in vacuo
  6. customThe crude product was purified on silica (75% DCM/hexanes)

出典と根拠

ORDレコード
ord-c446a2855e364668ba8487f6ba1bf70e
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879797B2

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