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Potassium Carbonate → Benzene, 5-methoxy-1,3-dimethyl-2-nitro-

HRID 1284962
ノート
印刷プレビュー

反応式

HRID 1284962 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:12])[CH:5]=[C:6]([CH3:11])[C:7]=1[N+:8]([O-:10])=[O:9].[CH3:13]C1C=CC(S(C)(=O)=O)=CC=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O.C(O)C>[CH3:11][C:6]1[CH:5]=[C:4]([O:12][CH3:13])[CH:3]=[C:2]([CH3:1])[C:7]=1[N+:8]([O-:10])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 18521p-Tolyl methyl sulfoneHCID 1384663,5-Dimethyl-4-nitrophenol

生成物 1

HCID 143760Benzene, 5-methoxy-1,3-dimethyl-2-nitro-

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

実験手順

3,5-dimethyl-4-nitrophenol (33.43 g), methyl p-toluene sulfonate (40.97 g) and K2CO3 (31.79 g) are stirred at reflux in 200 ml of acetone for four and one half hours and then stirred at R.T. overnight. The reaction mixture is filtered to give a dark amber filtrate. The filtrate is concentrated in vacuo to a yellowish brown solid which is dissolved in ethyl acetate washed with saturated aqueous sodium chloride, dried and concentrated in vacuo. The concentrate is distilled (87°-104° C./0.10 mm) to give a yellow waxy looking solid. The solid is dissolved in hot ethanol and recrystallized, M.P. 50°-52° C.

後処理

  1. filtrationThe reaction mixture is filtered
  2. customto give a dark amber filtrate
  3. concentrationThe filtrate is concentrated in vacuo to a yellowish brown solid which
  4. dissolutionis dissolved in ethyl acetate
  5. washwashed with saturated aqueous sodium chloride
  6. customdried
  7. concentrationconcentrated in vacuo
  8. distillationThe concentrate is distilled (87°-104° C./0.10 mm)
  9. customto give a yellow waxy
  10. customrecrystallized

出典と根拠

ORDレコード
ord-9624c1617f7c405aab115ce95d47a3cb
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04564640

反応ノート

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