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

Sodium Hydroxide → (4-Trifluoromethyl-phenyl)-{4-[1-(4-Methoxy2,3-Dimethyl-phenyl)-ethyl]-piperazin-1-yl}-methanone

HRID 967045
ノート
印刷プレビュー

反応式

HRID 967045 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH3:10])=[C:5]([CH3:17])[C:4]=1[CH3:18].[OH-].[Na+].[F:21][C:22]([F:33])([F:32])[C:23]1[CH:31]=[CH:30][C:26]([C:27](Cl)=[O:28])=[CH:25][CH:24]=1>C1(C)C=CC=CC=1>[F:21][C:22]([F:32])([F:33])[C:23]1[CH:24]=[CH:25][C:26]([C:27]([N:14]2[CH2:13][CH2:12][N:11]([CH:9]([C:6]3[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([CH3:18])[C:5]=3[CH3:17])[CH3:10])[CH2:16][CH2:15]2)=[O:28])=[CH:30][CH:31]=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 3

HCID 14798Sodium HydroxideHCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 220219311-[1-(4-Methoxy-2,3-dimethyl-phenyl)-ethyl]-piperazine

生成物 1

HCID 10136921(4-Trifluoromethyl-phenyl)-{4-[1-(4-Methoxy2,3-Dimethyl-phenyl)-ethyl]-piperazin-1-yl}-methanone

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1-[1-(4-Methoxy-2,3-dimethyl-phenyl)-ethyl]-piperazine (0.02 g, 0.081 mmole) was dissolved in anhydrous toluene and 1N NaOH (1:1) at room temperature. The 4-trifluoromethyl benzoyl chloride (0.013 ml, 0.081 mmole) was added into the reaction mixture. The reaction mixture was stirred at room temperature for 30 minutes. The mixture was washed with 1N NaOH, extracted with EtOAC. The combined organic layers were dried over MgSO4. After removal organic solvent, the residue was purified by SCX column eluted with MeOH and 10% MeOH (NH3) in dichloromethane. (4-Trifluoromethyl-phenyl)-{4-[1-(4-Methoxy2,3-Dimethyl-phenyl)-ethyl]-piperazin-1-yl}-methanone (compound 10) was obtained as a pale yellow oil (0.010 g 30%). Analysis H1 NMR (400MHz, CDCl3): 7.65 (2H, d), 7.495 (2H, d), 7.19 (1H, d), 6.689 (1H, d), 3.764 (3H, s), 3.682 (1H, q), 3.317 (2H, m), 2.506 (6H, m), 2.266 (3H, s), 2.164 (3H, s) 1.286 (3H, d). MS (LC-MS): Calculated for C23H27F3N2O2 420.47, found 421.26 (M+). XII. {5-[1-4-Methoxy-2,3-dimethyl-phenyl)-ethyl]-(1S,4S)-2,5-diaza-bicyclo[2.2.1]hept-2-yl}-(4-trifluoromethyl-phenyl)-methanone (compound 11)

後処理

  1. customat room temperature
  2. washThe mixture was washed with 1N NaOH
  3. extractionextracted with EtOAC
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. customAfter removal organic solvent
  6. customthe residue was purified by SCX column
  7. washeluted with MeOH and 10% MeOH (NH3) in dichloromethane

出典と根拠

ORDレコード
ord-38db3dd5c9b4441da58dd48fe029f78d
出典データセット
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06953801B2

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