Hydrogen Peroxide → 5-Fluoro-2-methyl-1-(p-methylsulfinylbenzyl)-indene

HRID 918296노트

반응식

HRID 918296 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7]([CH2:11][C:12]1[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][CH:13]=1)[C:6]([CH3:20])=[CH:5]2.C(Cl)(Cl)Cl.[OH:25]O>C(O)(=O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7]([CH2:11][C:12]1[CH:13]=[CH:14][C:15]([S:18]([CH3:19])=[O:25])=[CH:16][CH:17]=1)[C:6]([CH3:20])=[CH:5]2

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 6212ChloroformHCID 215218885-Fluoro-2-methyl-1-(p-methylthiobenzyl)-indene

생성물 1

HCID 215218865-Fluoro-2-methyl-1-(p-methylsulfinylbenzyl)-indene

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

500 mg. (1.755 mm) of 5-fluoro-2-methyl-1-(p-methylthiobenzyl)-indene is dissolved in 5 ml. of chloroform. To this solution is added 30% hydrogen peroxide (equivalent to 2.645 mm). The reaction mixture is aged for 1 hour at room temperature followed by the addition of 5 ml. of glacial acetic acid and aged for an additional hour. The reaction mixture is then diluted with 25 ml. of 1:1 benzene-ether and extracted with 6 × 25 ml. of 3% aqueous sodium chloride. The solution is then dried over sodium sulfate and evaporated in vacuo to yield an oil. Recrystallization from ice-cold isopropanol gives 5-fluoro-2-methyl-1-(p-methylsulfinylbenzyl)-indene.

후처리

  1. additionfollowed by the addition of 5 ml
  2. additionThe reaction mixture is then diluted with 25 ml
  3. extractionof 1:1 benzene-ether and extracted with 6 × 25 ml
  4. dry with materialThe solution is then dried over sodium sulfate
  5. customevaporated in vacuo
  6. customto yield an oil
  7. customRecrystallization from ice-cold isopropanol

출처 및 근거

ORD 기록
ord-77c1e49fd41b45d18dbfd6c8a7351f0b
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03970693

반응 노트

불러오는 중…