Carbon Dioxide → beta-Phenylisovaleric acid

HRID 495111

반응식

HRID 495111 반응식
[Mg].[CH2:2](Cl)[C:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:5])[CH3:4].BrCCBr.Cl.[C:18](=[O:20])=[O:19]>CC(OC)(C)C.O1CCCC1>[CH3:4][C:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:5])[CH2:2][C:18]([OH:20])=[O:19]

참가 물질

8

반응물 5

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 78391,2-DibromoethaneHCID 68191Neophyl chloride2회HCID 5462224Magnesium

생성물 1

HCID 13890beta-Phenylisovaleric acid

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 15413tert-Butyl methyl ether용매2회

실험 절차

Magnesium (4,86 g, 0.2 mol, 50-150 mesh), neophylchloride (0.2 g) and tetrahydrofurane(10 ml) were placed in a flask under an atmosphere of argon. A Grignard reaction was then started with 1,2-dibromoethane (0.2 ml). Neophylchloride (35,47 g, 0.2 mol) dissolved in MTBE (50 ml) was then added at reflux over a period of 50 minutes. After stirring for 2½ h at the same temperature, the reaction mixture was diluted with MTBE and dried CO2 was introduced above the surface at a temperature of 35° C. (ice cooling). The mixture was then acidified with HCl and extracted with MTBE. GC revealed the presence of 2,5-dimethyl-2,5-diphenyl-hexane and phenylisobutyric in a ratio of 54:46.

후처리

  1. customA Grignard reaction
  2. additionwas then added
  3. temperatureat reflux over a period of 50 minutes
  4. additionwas introduced above the surface at a temperature of 35° C. (ice cooling)
  5. extractionextracted with MTBE

출처 및 근거

ORD 기록
ord-8f474afbc12f4e07bfccb7a52cd11650
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538243B2

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