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Benzyl Bromide → Benzyl 2-methoxy-3-nitrobenzoate

HRID 2423237
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HRID 2423237 반응식
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:15][O:16][C:17]1[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][CH:23]=[CH:22][C:18]=1[C:19]([OH:21])=[O:20]>CN(C=O)C>[CH3:15][O:16][C:17]1[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][CH:23]=[CH:22][C:18]=1[C:19]([O:21][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 120151952-Methoxy-3-nitrobenzoic acid

생성물 1

HCID 67246088Benzyl 2-methoxy-3-nitrobenzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

At room temperature, benzyl bromide (8.85 mL) and potassium carbonate (10.3 g) were added to a DMF (150 mL) solution of 2-methoxy-3-nitrobenzoic acid (9.80 g), followed by stirring for 70 minutes. The insoluble matter was separated by filtration, followed by evaporation under reduced pressure. This was subjected to liquid-liquid separation with ethyl acetate, aqueous sodium hydrogencarbonate solution, and hexane added thereto. The organic layer was washed with water and saturated brine in that order, dried, and then evaporated under reduced pressure to obtain benzyl 2-methoxy-3-nitrobenzoate (14.3 g).

후처리

  1. customThe insoluble matter was separated by filtration
  2. customfollowed by evaporation under reduced pressure
  3. customThis was subjected to liquid-liquid separation with ethyl acetate, aqueous sodium hydrogencarbonate solution, and hexane
  4. additionadded
  5. washThe organic layer was washed with water and saturated brine in that order
  6. customdried
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-75956b4746904735a1e1ff72c34da9c7
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960562B2

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