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Dimethyl malonate → HCID 18626507, 화합물

HRID 368335
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HRID 368335 반응식
[C:1]([O:8][CH3:9])(=[O:7])[CH2:2][C:3]([O:5][CH3:6])=[O:4].[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:17]=[CH:18][C:19]=1[CH3:20])[CH2:15]Br>CO>[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:17]=[CH:18][C:19]=1[CH3:20])[CH2:15][CH:2]([C:1]([O:8][CH3:9])=[O:7])[C:3]([O:5][CH3:6])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7943Dimethyl malonateHCID 185096604-(bromomethyl)-2-methoxy-1-methylbenzene

생성물 1

HCID 18626507HCID 18626507, 화합물수율 95.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 2.6 g (0.1124 g-atom) of Na in 50 mL of MeOH was treated with 12.9 mL (0.1124 mol) of dimethyl malonate and allowed to stir for 45 minutes. This was then treated dropwise with 24.17 g (0.1124 mol) of 3-methoxy-4-methylbenzyl bromide and the solution heated at reflux overnight. The solvent was removed under reduced pressure and the residue taken up in EtOAc. This was washed with 6% HCl, H2O, saturated NaHCO3, and saturated NaCl. Drying over MgSO4 and removal of the solvent under reduced pressure gave 28.54 g (95.5% yield) of the product as a pale yellow oil. The structure was confirmed by NMR spectroscopy.

후처리

  1. temperaturethe solution heated
  2. temperatureat reflux overnight
  3. customThe solvent was removed under reduced pressure
  4. washThis was washed with 6% HCl, H2O, saturated NaHCO3, and saturated NaCl
  5. dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-ef320f77968a45e69988338a2c03cac8
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06133303

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