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

HRID 1869785

반응식

HRID 1869785 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-77af4de373604e2a9cb8fa413103c2c6
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638630B2

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