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

HRID 978013ノート

反応式

HRID 978013 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6cde466ae0a4e39bd14a6372ab7f4ec
出典データセット
uspto-grants-1987_05
特許番号
US04663320

反応ノート

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