Water → 4-Methoxyresorcinol

HRID 1184970

반응식

HRID 1184970 반응식
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11]C=O)=[CH:7][C:6]=1[O:14]C)(=O)C.O.[Li+].[OH-]>C1COCC1>[CH3:1][O:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[OH:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 866739234-(Formyloxy)-2-methoxyphenyl acetate

생성물 1

HCID 30839364-Methoxyresorcinol수율 45.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-(formyloxy)-2-methoxyphenyl acetate (16 g, 76 mmol) in THF (50 mL)/H2O (50 mL) was added LiOH (7.7 g, 184.2 mmol). The reaction was stirred at room temperature overnight. The volatiles were removed under reduced pressure. The residue was extracted with EA (50 mL×3). The organic phase was washed with brine (50 mL), dried over Na2SO4, filtrated and concentrated in vacuo to give black oil, which was purified by silica gel column (PE:EA=3:1) to afford 4.8 g of product (40%) as a brown solid.

후처리

  1. customThe volatiles were removed under reduced pressure
  2. extractionThe residue was extracted with EA (50 mL×3)
  3. washThe organic phase was washed with brine (50 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltrated
  6. concentrationconcentrated in vacuo
  7. customto give black oil, which
  8. customwas purified by silica gel column (PE:EA=3:1)

출처 및 근거

ORD 기록
ord-273f2c5841054f85819cc10e0b4dadeb
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08669381B2

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