Ethyl Acetate → HCID 22633147, 화합물

HRID 2417385노트

반응식

HRID 2417385 반응식
[C:1]([O:4][C:5]1[C:12]([O:13][CH3:14])=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][C:6]=1[O:15][CH3:16])(=[O:3])[CH3:2].[Br:17]Br.C(OCC)(=O)C>C(O)(=O)C.O>[C:1]([O:4][C:5]1[C:12]([O:13][CH3:14])=[CH:11][C:8]([CH:9]=[O:10])=[C:7]([Br:17])[C:6]=1[O:15][CH3:16])(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 24408BromineHCID 6881894-Acetoxy-3,5-dimethoxybenzaldehyde

생성물 1

HCID 22633147HCID 22633147, 화합물수율 92.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

To a mixture of 4-acetoxy-3,5-dimethoxy benzaldehyde (5.4 g, 20 mmol) and 5.4 g (40 mmol) of NaOAc.3H2O in acetic acid (14 mL) and water (2 mL) was added dropwise bromine (1.2 mL, 24 mmol). The mixture was stirred at RT overnight and repartitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate (3×) and the combined organic layer was washed with saturated sodium bicarbonate solution, water and brine and dried over anhydrous sodium sulfate. Removal of the solvent gave 5.6 g of 4-acetoxy-2-bromo-3,5-dimethoxybenzaldehyde (80%).

후처리

  1. extractionThe aqueous layer was extracted with ethyl acetate (3×)
  2. washthe combined organic layer was washed with saturated sodium bicarbonate solution, water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-40e2b32a56374d41af71a5110c0d8cbe
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825208B2

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