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

HRID 581170

반응식

HRID 581170 반응식
[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]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 120695-Nitroisophthalic acid

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5753f5aef7c3445caa610b07a58cadb6
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919829

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