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Propionic Acid → N-({2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-(tri-fluoromethyl)pyrimidin-5-yl}methyl)propanamide

HRID 918769
ノート
印刷プレビュー

反応式

HRID 918769 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2([C:27]([F:30])([F:29])[F:28])[CH2:14][CH2:13][N:12]([C:15]3[N:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[C:18]([CH2:25][NH2:26])=[CH:17][N:16]=3)[CH2:11]2)[CH:5]=[C:6]([Cl:9])[C:7]=1[Cl:8].C(N(CC)CC)C.[C:38](O)(=[O:41])[CH2:39][CH3:40]>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2([C:27]([F:28])([F:29])[F:30])[CH2:14][CH2:13][N:12]([C:15]3[N:20]=[C:19]([C:21]([F:23])([F:24])[F:22])[C:18]([CH2:25][NH:26][C:38](=[O:41])[CH2:39][CH3:40])=[CH:17][N:16]=3)[CH2:11]2)[CH:5]=[C:6]([Cl:9])[C:7]=1[Cl:8]
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 1032Propionic AcidHCID 8471TriethylamineHCID 594533771-{2-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidin-5-yl}methanamine

生成物 1

HCID 45378076N-({2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-(tri-fluoromethyl)pyrimidin-5-yl}methyl)propanamide収率 90%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

1-{2-[3-(3,4,5-Trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidin-5-yl}methanamine (0.1 g) and triethylamine (0.05 g) were added to dichloromethane (20 mL), and then dichloromethane solution (10 mL) comprising anhydrous propionic acid (0.05 g) was added dropwise thereto under ice cooling. After the dropwise addition was completed, the reaction solution was stirred at room temperature for one hour. The solvent was evaporated off under reduced pressure, and the residue was then purified by a silica gel chromatography to obtain the title compound (0.1 g, 90%).

後処理

  1. additionAfter the dropwise addition
  2. customThe solvent was evaporated off under reduced pressure
  3. customthe residue was then purified by a silica gel chromatography

出典と根拠

ORDレコード
ord-b7a403057edf4756a922824cd0ce264b
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09271499B2

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