Ethyl Bromide → 2-Ethoxy-1-methoxy-4-nitro-benzene

HRID 1162189노트

반응식

HRID 1162189 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:4]=1[OH:12].C([O-])([O-])=O.[K+].[K+].[CH2:19](Br)[CH3:20]>CN(C=O)C.CCOC(C)=O>[CH2:19]([O:12][C:4]1[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1])[CH3:20]

참가 물질

6

반응물 3

HCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 694712-Methoxy-5-nitrophenol

생성물 1

HCID 117901432-Ethoxy-1-methoxy-4-nitro-benzene

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
40 °C

실험 절차

2-methoxy-5-nitro-phenol (508 mg, 3 mmoles) was dissolved in DMF (20 mL) under nitrogen atmosphere. K2CO3 (900 mg, 6.5 mmoles), KI (490 mg, 2.95 mmol) and ethyl bromide (0.250 mL, 3.3 mmoles) were added, and the suspension was heated to 40° C. for 28 hours. The mixture was diluted with AcOEt (60 mL) and extracted with 1N NaOH (40 mL) and water (40 mL). The organic layer was dried over Na2SO4 and evaporated to dryness. The crude was employed in the next step without purification.

후처리

  1. extractionextracted with 1N NaOH (40 mL) and water (40 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customevaporated to dryness
  4. customThe crude was employed in the next step without purification

출처 및 근거

ORD 기록
ord-5b71ee367d584600828d1754b4ae04ae
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820698B2

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