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

HRID 1451639ノート

反応式

HRID 1451639 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 2723922Sodium ethoxide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-78659a571efd4bcf9572276fb9e0cf58
出典データセット
uspto-grants-1997_02
特許番号
US05604237

反応ノート

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