Dimethyl 2-(4-chloro-2-nitrophenyl)malonate → Methyl 2-(4-chloro-2-nitrophenyl)acetate

HRID 1827450노트

반응식

HRID 1827450 반응식
[CH3:1][O:2][C:3](=[O:19])[CH:4]([C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=1[N+:16]([O-:18])=[O:17])C(OC)=O>O.CN1C(=O)CCC1>[CH3:1][O:2][C:3](=[O:19])[CH2:4][C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=1[N+:16]([O-:18])=[O:17]

참가 물질

4

반응물 1

HCID 2727544Dimethyl 2-(4-chloro-2-nitrophenyl)malonate

생성물 1

HCID 10944246Methyl 2-(4-chloro-2-nitrophenyl)acetate수율 102.6%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A solution of 2-(4-Chloro-2-nitro-phenyl)-malonic acid dimethyl ester (195 g, 679.4 mmol) in water (100 mL) and NMP (1000 mL) was heated to reflux for 3.5 hours. The solvent was removed by rotary evaporation to an oil. The oil was dissolved in EtOAc, and then washed with water (5×300 mL). The aqueous layer was then extracted with EtOAc (4×300 mL). The organic was washed with water. The organic layers were combined and dried over MgSO4. After removing the solids by filtration, the solvent was evaporated to yield the desired product as a orange/brown solid (160.0 g, 95%).

후처리

  1. temperatureto reflux for 3.5 hours
  2. customThe solvent was removed by rotary evaporation to an oil
  3. dissolutionThe oil was dissolved in EtOAc
  4. washwashed with water (5×300 mL)
  5. extractionThe aqueous layer was then extracted with EtOAc (4×300 mL)
  6. washThe organic was washed with water
  7. dry with materialdried over MgSO4
  8. customAfter removing the solids
  9. filtrationby filtration
  10. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-106b3696d95248948686785afde073a1
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07053107B2

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