Potassium Carbonate → Methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate

HRID 1869785

反応式

HRID 1869785 の反応式
[NH2:1][CH:2]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)[C:3]([O:5][CH3:6])=[O:4].C([O-])([O-])=O.[K+].[K+].[Cl:23][C:24]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[C:25]=1[CH2:26]Br>CC#N>[Cl:23][C:24]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[C:25]=1[CH2:26][NH:1][CH:2]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)[C:3]([O:5][CH3:6])=[O:4]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 301591-Bromomethyl-2,6-dichlorobenzeneHCID 560520Methyl 2-amino-3-(4-nitrophenyl)propanoate

生成物 1

HCID 11269078Methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of methyl 2-amino-3-(4-nitrophenyl)propanoate 2 (6 g) in CH3CN (30 ml) is added, pulverized K2CO3 (11.095 g), 2,6-dichlorobenzyl bromide (6.42 g). The mixture is stirred at RT for 6 h then filtrated on decalite and evaporated. The residue is placed in CH2Cl2 (100 ml) and washed three time with water (100 ml) dried over MgSO4 and evaporated. The residue is purified by silica gel chromatography using AcOEt/hexane 10/90 as eluent.

後処理

  1. filtrationthen filtrated on decalite
  2. customevaporated
  3. washwashed three time with water (100 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe residue is purified by silica gel chromatography

出典と根拠

ORDレコード
ord-77af4de373604e2a9cb8fa413103c2c6
出典データセット
uspto-grants-2009_12
特許番号
US07638630B2

関連ノート

読み込み中…