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Isobutylene → HCID 22261682, 화합물

HRID 413427
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HRID 413427 반응식
[CH2:1]([O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:11])[CH:6]=1)[CH3:2].[CH3:13][C:14](=[CH2:16])[CH3:15].OS(C(F)(F)F)(=O)=O.CCN(CC)CC>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:14]([CH3:16])([CH3:15])[CH3:13])[CH:6]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8255IsobutyleneHCID 8471TriethylamineHCID 24522Ethyl 3-hydroxybenzoateHCID 62406Trifluoromethanesulfonic acid

생성물 1

HCID 22261682HCID 22261682, 화합물수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
-20 °C

실험 절차

Into a solution of 3-hydroxy-benzoic acid ethyl ester (10.14 g, 0.061 mol) in CH2Cl2 (200 mL) cooled to −78° C. was condensed isobutylene (150 mL) followed by addition of triflic acid (1.08 mL, 0.061 mol). The reaction mixture was allowed to warm to −20° C. When a solution was obtained and tlc indicated loss of starting material, the reaction was quenched with Et3N (6.8 mL, 0.049 mol) and left to warm to ambient temperature. The solution was concentrated and the residue chromatographed on an ISCO combiflash eluting with 0-10% EtoAc/hexane to give 12.91 g (95%) of the title compound.

후처리

  1. customWhen a solution was obtained
  2. waitleft
  3. temperatureto warm to ambient temperature
  4. concentrationThe solution was concentrated
  5. customthe residue chromatographed on an ISCO combiflash
  6. washeluting with 0-10% EtoAc/hexane

출처 및 근거

ORD 기록
ord-d398883e6780446f99684757957ae474
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06566385B2

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