Hydrochloric Acid → 4-(3-Formyl-4-nitro-phenoxy)-butyric acid

HRID 1154599노트

반응식

HRID 1154599 반응식
[CH:1]([C:3]1[CH:4]=[C:5]([O:12][CH2:13][CH2:14][CH2:15][C:16]([O:18]CC)=[O:17])[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10])=[O:2].[OH-].[Na+].Cl.CCOCC>C(O)C>[CH:1]([C:3]1[CH:4]=[C:5]([O:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17])[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10])=[O:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 10588876Ethyl 4-((3-formyl-4-nitrophenyl)oxy)butyrate

생성물 1

HCID 27592274-(3-Formyl-4-nitro-phenoxy)-butyric acid수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of ethyl 4-(3-formyl-4-nitrophenyl)oxybutyrate (65 g) in ethanol (400 ml) was added 3N NaOH (100 ml) in small portions. After 30 minutes at room temperature the reaction mixture was acidified with concentrated HCl and the ethanol evaporated. The aqueous residue was extracted with ethyl acetate (4×200 ml). The combined organic layers were washed with brine (2×200 ml), dried over Na2SO4, filtered and evaporated to give a light yellow solid. Trituration with ether afforded 4-(3-formyl-4-nitrophenyl)oxybutyric acid (55 g), m.p. 109°-110° C.

후처리

  1. customthe ethanol evaporated
  2. extractionThe aqueous residue was extracted with ethyl acetate (4×200 ml)
  3. washThe combined organic layers were washed with brine (2×200 ml)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give a light yellow solid

출처 및 근거

ORD 기록
ord-76da3dd575094b4e9dcdbce8b3a96605
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490371

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