Sulfuric Acid → 1,3-di-tert-Butyl 5-nitrobenzene-1,3-dicarboxylate

HRID 581170

反応式

HRID 581170 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=[O:14])[CH:7]=[C:8]([CH:12]=1)[C:9]([OH:11])=[O:10])([O-:3])=[O:2].S(=O)(=O)(O)O.[CH3:21][C:22](=[CH2:24])[CH3:23]>ClCCl>[C:22]([O:10][C:9]([C:8]1[CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=[C:6]([C:13]([O:15][C:6]([CH3:13])([CH3:7])[CH3:5])=[O:14])[CH:7]=1)=[O:11])([CH3:23])([CH3:21])[CH3:24]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 120695-Nitroisophthalic acid

生成物 1

HCID 540121621,3-di-tert-Butyl 5-nitrobenzene-1,3-dicarboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5-Nitroisophthalic acid (4.22 g, 20 mmol) was suspended in dichloromethane (80 ml) and concentrated sulphuric acid (1 ml) was added. The solution was stirred and then saturated with isobutylene gas. The reaction vessel was stoppered and stirred at room temperature overnight. The solution was filtered and anhydrous potassium carbonate was added to the filtrate. the solution was filtered and evsaporated and the residue recrystallised from ethanol to leave the title compound as a white solid (2.2 g).

後処理

  1. stirringstirred at room temperature overnight
  2. filtrationThe solution was filtered
  3. additionanhydrous potassium carbonate was added to the filtrate
  4. filtrationthe solution was filtered
  5. customthe residue recrystallised from ethanol

出典と根拠

ORDレコード
ord-5753f5aef7c3445caa610b07a58cadb6
出典データセット
uspto-grants-1999_07
特許番号
US05919829

関連ノート

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