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Hydrochloric Acid → 5-(3,4-Dimethoxyphenyl)-5-oxovaleric acid

HRID 1088860
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HRID 1088860 반응식
[C:1]1([O:9][CH3:10])[C:2](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O:3][CH3:4].[C:11]1(=[O:18])[O:17][C:15](=[O:16])[CH2:14][CH2:13][CH2:12]1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>[N+](C1C=CC=CC=1)([O-])=O>[CH3:4][O:3][C:2]1[CH:5]=[C:6]([C:11](=[O:18])[CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])[CH:7]=[CH:8][C:1]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7043VeratroleHCID 7940Glutaric anhydrideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 27584705-(3,4-Dimethoxyphenyl)-5-oxovaleric acid

시약·촉매·용매 1

HCID 7416Nitrobenzene용매2회

실험 절차

A solution containing 36 g of veratrole and 30 g glutaric anhydride in 120 ml of nitrobenzene was gradually added while stirring and cooling at 0° C. to a mixture of 72 g of anhydrous aluminium chloride and 240 ml of nitrobenzene. The mixture was stirred for 1 h at 0° C. and then for 18 h at 20° C. Ice and hydrochloric acid were added to the reaction mixture. Nitrobenzene layer was separated and to this ethyl acetate was added whereupon the product crystallized. After filtering the crystals were washed with ethyl acetate. Yield 42.3 g (64%).

후처리

  1. additionwas gradually added
  2. stirringThe mixture was stirred for 1 h at 0° C.
  3. customNitrobenzene layer was separated and to this ethyl acetate
  4. additionwas added whereupon the product
  5. customcrystallized
  6. filtrationAfter filtering the crystals
  7. washwere washed with ethyl acetate

출처 및 근거

ORD 기록
ord-45eb9fac1f024a4fb90f0660f36755c9
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04963590

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