p-Toluenesulfonic acid → Isobutyl acetoacetate

HRID 2845

반응식

HRID 2845 반응식
[C:1](OCC)(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:21]([OH:25])[CH:22]([CH3:24])[CH3:23]>>[C:1]([O:25][CH2:21][CH:22]([CH3:24])[CH3:23])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4]

참가 물질

4

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 6560IsobutanolHCID 8868Ethyl Acetoacetate

생성물 1

HCID 522677Isobutyl acetoacetate

실험 절차

30 ml of ethyl acetoacetate were dissolved in 350 ml of i-butyl alcohol and a catalytic amount of p-toluensulphonic acid (PTSA) was added. The solution was refluxed for 18 h. The reaction mixture was evaporated in vacuo and the residue was dissolved in ether. The resulted solution was treated with s.s. NaHCO3. The organic layer was separated, dried over Na2SO4 and evaporated in vacuo. The crude oil was distilled at 66°-68° C./4 mmHg, to give 18.8 g of the title compound.

후처리

  1. temperatureThe solution was refluxed for 18 h
  2. customThe reaction mixture was evaporated in vacuo
  3. dissolutionthe residue was dissolved in ether
  4. additionThe resulted solution was treated with s.s
  5. customThe organic layer was separated
  6. dry with materialdried over Na2SO4
  7. customevaporated in vacuo
  8. distillationThe crude oil was distilled at 66°-68° C./4 mmHg

출처 및 근거

ORD 기록
ord-78feaec48f454c398ecf0ddf11da5e02
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731322

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