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

p-Toluenesulfonic acid → 1-(3-Dimethylaminophenyl)-2-methyl-5-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester

HRID 413885
ノート
印刷プレビュー

反応式

HRID 413885 の反応式
Cl.Cl.[CH3:3][N:4]([CH3:12])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([NH2:11])[CH:6]=1.C(N(CC)CC)C.[CH2:20]([O:22][C:23](=[O:37])[CH:24]([CH2:28][C:29](=O)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:25](=O)[CH3:26])[CH3:21].CC1C=CC(S(O)(=O)=O)=CC=1>C(O)C>[CH2:20]([O:22][C:23]([C:24]1[CH:28]=[C:29]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[N:11]([C:7]2[CH:8]=[CH:9][CH:10]=[C:5]([N:4]([CH3:12])[CH3:3])[CH:6]=2)[C:25]=1[CH3:26])=[O:37])[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

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 8471TriethylamineHCID 771241,3-Benzenediamine, N1,N1-dimethyl-, hydrochloride (1:2)HCID 312893Ethyl 2-acetyl-4-oxo-4-phenylbutanoate

生成物 1

HCID 101324961-(3-Dimethylaminophenyl)-2-methyl-5-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

N,N-dimethyl-1,3-phenylenediamine dihydrochloride (5 mmol, 1.0 g), triethylamine (10 mmol, 1.4 mL), 3-oxo-2-(2-oxo-2-phenyl-ethyl)-butyric acid ethyl ester (5 mmol, 1.2 g), and tosic acid (0.1 g) were combined in ethanol (25 mL), then heated under reflux (12 hrs). The solvents were removed under vacuum, the resulting oil was redissolved in methylene chloride, then applied to a silica column. The purified product was collected as a translucent oil. The named compound was identified by 1H-NMR (CDCl3, ppm): 1.28 t (3H), 2.35 s (3H), 2.77 s (6H), 4.2 q (2H), 6.3-6.7 m (4H), and 7.0-7.3 m (5H).

後処理

  1. temperatureheated
  2. temperatureunder reflux (12 hrs)
  3. customThe solvents were removed under vacuum
  4. dissolutionthe resulting oil was redissolved in methylene chloride
  5. customThe purified product was collected as a translucent oil

出典と根拠

ORDレコード
ord-1018c1edffcf433f8cded781d00d00c1
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06569890B2

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