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N-Methylbenzylamine → 2-[Benzyl(methyl)amino]-1-(4-fluorophenyl)ethan-1-one

HRID 1351252
ノート
印刷プレビュー

反応式

HRID 1351252 の反応式
[CH2:1]([NH:8][CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl[CH2:18][C:19]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)=[O:20].C(OCC)(=O)C>CN(C)C=O>[CH2:1]([N:8]([CH3:9])[CH2:18][C:19]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 7669N-MethylbenzylamineHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 1202482-Chloro-4'-fluoroacetophenone

生成物 1

HCID 144592512-[Benzyl(methyl)amino]-1-(4-fluorophenyl)ethan-1-one収率 95.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

To a solution of benzyl-methyl-amine (28.9 g) and triethylamine (33.8 mL) in dimethylformamide (600 mL) was added in 5 portions 2-chloro-1-(4-fluorophenyl)-ethanone (40 g) on an ice bath. After stirring at room temperature for 2 hours, ethyl acetate was added, and the salt that precipitated was removed by filtration, and the filtrate was concentrated. A crude purification was carried out by silica gel column chromatography (hexane/ethyl acetate), and the title compound (56.9 g) was obtained as a colorless oily matter.

後処理

  1. customthe salt that precipitated
  2. customwas removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customA crude purification

出典と根拠

ORDレコード
ord-5ae767fe029b4d3ab468b43f9e5694cf
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07217723B2

反応ノート

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