P-Xylene → 2-(2,5-Dimethylphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol

HRID 1675646노트

반응식

HRID 1675646 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[CH:6][CH:7]=1.[F:9][C:10]([F:18])([F:17])[C:11]([C:13]([F:16])([F:15])[F:14])=[O:12]>[Cl-].[Al+3].[Cl-].[Cl-].Cl>[F:9][C:10]([F:18])([F:17])[C:11]([C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[CH3:1])([OH:12])[C:13]([F:16])([F:15])[F:14]

참가 물질

5

반응물 2

HCID 7809P-XyleneHCID 12695Hexafluoroacetone

생성물 1

HCID 27750852-(2,5-Dimethylphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol수율 88.2%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 313Hydrochloric Acid용매

실험 절차

A 1 L reactor was charged under nitrogen with 200.0 g (1.88 mol) of p-xylene and 12.5 g (0.094 mol/0.06 eq) of aluminum chloride, followed by adjusting the inside temperature to 18° C. Then, 327.7 g (1.97 mol/1.06 eq) of hexafluoroacetone was introduced in a temperature range of 18-25° C. After the introduction, stirring was conducted at room temperature for 3 hr. Then, 200 mL of 10% hydrochloric acid was added. The resulting aqueous layer was extracted two times with 50 mL of chloroform. The resulting organic layers were combined together, followed by removing water with anhydrous magnesium sulfate, filtration, concentration, and vacuum distillation, thereby obtaining 451.3 g of 2-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]-1,4-dimethylbenzene represented by the following formula. Upon this, purity was 92%, and yield was 81%.

후처리

  1. customto 18° C
  2. extractionThe resulting aqueous layer was extracted two times with 50 mL of chloroform
  3. customby removing water
  4. filtrationwith anhydrous magnesium sulfate, filtration, concentration, and vacuum distillation

출처 및 근거

ORD 기록
ord-e5287b55771349f9ae31046cec9ec7a3
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003749B2

반응 노트

불러오는 중…