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

Trifluoroacetic acid → 2-(4,4-Dimethyl-1,1-dioxido-1,2,5-thiadiazolidin-2-yl)-4-fluorobenzonitrile

HRID 1093038
ノート
印刷プレビュー

反応式

HRID 1093038 の反応式
[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N:10]2[CH2:14][C:13]([CH3:16])([CH3:15])[N:12](CC3C=CC(OC)=CC=3)[S:11]2(=[O:27])=[O:26])[CH:3]=1.FC(F)(F)C(O)=O>ClCCl.CO>[CH3:15][C:13]1([CH3:16])[NH:12][S:11](=[O:27])(=[O:26])[N:10]([C:4]2[CH:3]=[C:2]([F:1])[CH:9]=[CH:8][C:5]=2[C:6]#[N:7])[CH2:14]1
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 2

HCID 6422Trifluoroacetic acidHCID 579051604-Fluoro-2-(5-(4-methoxybenzyl)-4,4-dimethyl-1,1'-dioxido-1,2,5-thiadiazolidin-2-yl)benzonitrile

生成物 1

HCID 579049732-(4,4-Dimethyl-1,1-dioxido-1,2,5-thiadiazolidin-2-yl)-4-fluorobenzonitrile収率 100%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-fluoro-2-(5-(4-methoxybenzyl)-4,4-dimethyl-1,1′-dioxido-1,2,5-thiadiazolidin-2-yl)benzonitrile (4.6 g, 11.81 mmol) in dichloromethane (30 mL) was added trifluoroacetic acid (2.73 mL, 35.4 mmol) and the mixture stirred at room temperature for 18 h. The mixture was diluted with methanol and the white solid collected by filtration and discarded. The cloudy solution was concentrated and the resulting solid was triturated with methanol and then filtered to give the title compound as a white solid (3.18 g, 100% yield). LCMS (M+H) calcd for C11H13FN3O2S: 270.07; found: 270.00. 1H NMR (300 MHz, CDCl3) δ: 7.66 (0.2H, dd, J=8.8, 5.8 Hz), 7.58 (1H, dd, J=9.5, 2.6 Hz), 7.10-7.04 (1H, m), 4.48 (1H, brs), 3.85 (2H, s), 1.55 (6H, s).

後処理

  1. filtrationthe white solid collected by filtration
  2. concentrationThe cloudy solution was concentrated
  3. customthe resulting solid was triturated with methanol
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-0a88495e7be64b26a1e9c634181295db
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129398B2

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