Diethyl Malonate → Diethyl (3-methyl-4-nitrobenzyl)malonate

HRID 1451639노트

반응식

HRID 1451639 반응식
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH3:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][C:20]=1[N+:21]([O-:23])=[O:22])[CH2:16]Br>C([O-])C.[Na+]>[CH3:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][C:20]=1[N+:21]([O-:23])=[O:22])[CH2:16][CH:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:1]([O:9][CH2:10][CH3:11])=[O:8]

참가 물질

4

반응물 2

HCID 7761Diethyl MalonateHCID 44459783-Methyl-4-nitrobenzyl bromide

생성물 1

HCID 54253538Diethyl (3-methyl-4-nitrobenzyl)malonate

시약·촉매·용매 1

HCID 2723922Sodium ethoxide용매

실험 절차

To a solution of sodium ethanolate [prepared from 1.35 g Na in ethanol (30 ml)] were added diethyl malonate (9.2 ml) and then dropwise 3-methyl-4-nitrobenzyl bromide (13.4 g). The mixture was stirred 30 minutes at room temperature, then 30 minutes under reflux and then concentrated. The residue is treated with water and hexane, the precipitate filtered and the filtrate extracted with diethyl ether. The organic extract was dried on sodium sulfate and concentrate to give the title compound as an oil (4 g).

후처리

  1. temperature30 minutes under reflux
  2. concentrationconcentrated
  3. additionThe residue is treated with water and hexane
  4. filtrationthe precipitate filtered
  5. extractionthe filtrate extracted with diethyl ether
  6. extractionThe organic extract
  7. customwas dried on sodium sulfate
  8. concentrationconcentrate

출처 및 근거

ORD 기록
ord-78659a571efd4bcf9572276fb9e0cf58
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604237

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