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

Triethylamine → N-[2-methoxy(methyl)amino-2-oxoethyl]-2-(trifluoromethyl)benzamide

HRID 56033
ノート
印刷プレビュー

反応式

HRID 56033 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[C:5]([NH:7][CH2:8][C:9]([OH:11])=[O:10])=[O:6].Cl.[CH3:19][NH:20]OC.Cl.[CH3:24]N(C)CCCN=C=NCC.C(N(CC)CC)C>ClCCl.CN(C)C1C=CN=CC=1>[CH3:24][O:10][C:9](=[O:11])[CH:8]([NH:20][CH3:19])[NH:7][C:5](=[O:6])[C:4]1[CH:12]=[CH:13][CH:14]=[CH:15][C:3]=1[C:2]([F:16])([F:17])[F:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 167778182-((2-(Trifluoromethyl)phenyl)formamido)acetic acid

生成物 1

HCID 118071607N-[2-methoxy(methyl)amino-2-oxoethyl]-2-(trifluoromethyl)benzamide収率 59.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To 45.2 g of 2-[2-(trifluoromethyl)benzoylamino]acetic acid in 609 ml of dichloromethane, 21.4 g of N,O-dimethylhydroxylamine hydrochloride, 42.0 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 73.8 g of triethylamine and 2.2 g of 4-(dimethylamino)pyridine were added, and the mixture was stirred at room temperature for 18 hours. After completion of the reaction, the reaction mixture was washed with 500 ml of saturated anhydrous sodium hydrogen carbonate, 500 ml of 1N aqueous hydrochloric acid twice and 500 ml of water in this order, the resulting organic layer was dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was washed with 200 ml of hexane to obtain 31.4 g of the desired product as white crystals.

後処理

  1. customAfter completion of the reaction
  2. washthe reaction mixture was washed with 500 ml of saturated anhydrous sodium hydrogen carbonate, 500 ml of 1N aqueous hydrochloric acid twice
  3. dry with material500 ml of water in this order, the resulting organic layer was dried over saturated aqueous sodium chloride
  4. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
  5. washThe resulting residue was washed with 200 ml of hexane

出典と根拠

ORDレコード
ord-fc3ce71d56534995bb824e7f99629d9f
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434684B2

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