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

HRID 1162189ノート

反応式

HRID 1162189 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5b71ee367d584600828d1754b4ae04ae
出典データセット
uspto-grants-2010_10
特許番号
US07820698B2

反応ノート

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