Hydrochloric Acid → 4-Formyl-3-hydroxyphenyl acetate

HRID 2369828노트

반응식

HRID 2369828 반응식
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[O:12])=[C:7]([O:13]C(=O)C)[CH:6]=1)(=[O:3])[CH3:2].[OH-].[Na+].Cl>C(O)C.O.C(OCC)(=O)C>[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[O:12])=[C:7]([OH:13])[CH:6]=1)(=[O:3])[CH3:2]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11127858HCID 11127858, 화합물

생성물 1

HCID 126480914-Formyl-3-hydroxyphenyl acetate수율 44.5%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-formylbenzene-1,3-diyl diacetate (5.56 g, 25.08 mmol) in ethanol (20 mL) was added a solution of sodium hydroxide (1.00 g, 25.08 mmol) in water (12 mL). The reaction was stirred overnight at room temperature. The reaction was carefully neutralized with 2.0 N aqueous solution of hydrochloric acid (12.8 mL) at 0° C. and diluted with ethyl acetate (400 mL). The organic layer was washed with water (60 mL) and saturated aqueous sodium chloride (50 mL), dried over magnesium sulfate, filtered, and concentrated to afford, the product (2.01 g, 44% yield) as a gray solid: 1H NMR (400 MHz, d-MeOH): δ 9.90 (s, 1H), 7.68 (d, 1H), 6.80 (d, 1H), 6.75 (s, 1H), 4.82 (br s, 1H), 2.20 (s, 3H).

후처리

  1. washThe organic layer was washed with water (60 mL) and saturated aqueous sodium chloride (50 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto afford

출처 및 근거

ORD 기록
ord-2c2c921313354294946711a8f50c7eb3
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710038B2

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