Hydrogen iodide → Indane-1,3-dione, 2-(3-hydroxyphenyl)-

HRID 326437

반응식

HRID 326437 반응식
I.C[O:3][C:4]1[CH:5]=[C:6]([CH:10]2[C:18](=[O:19])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]2=[O:20])[CH:7]=[CH:8][CH:9]=1>C(Cl)(Cl)Cl>[OH:3][C:4]1[CH:5]=[C:6]([CH:10]2[C:11](=[O:20])[C:12]3[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:18]2=[O:19])[CH:7]=[CH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 24841Hydrogen iodideHCID 28178101H-Indene-1,3(2H)-dione, 2-(3-methoxyphenyl)-

생성물 1

HCID 617192Indane-1,3-dione, 2-(3-hydroxyphenyl)-

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
20 °C

실험 절차

Hydroiodic acid (50%, 205 parts) was added to 2-(3-methoxyphenyl)-1,3-indandione (67.1 parts) and the mixture was stirred under reflux for 10 minutes. By-product methyl iodide was removed by distillation and the solution was cooled to 20° C. The aqueous layer was decanted to leave a red oil. The oil was dissolved in chloroform (250 parts), washed with water (100 parts), separated and dried over anhydrous magnesium sulphate. The chloroform was removed by evaporation under reduced pressure to leave an orange solid. The solid was crystallised from toluene (1800 parts) to yield 2-(3-hydroxyphenyl)-1,3-indandione (30.6 parts), m.pt. 139°-141° C.

후처리

  1. temperatureunder reflux for 10 minutes
  2. customBy-product methyl iodide was removed by distillation
  3. customThe aqueous layer was decanted
  4. customto leave a red oil
  5. washwashed with water (100 parts)
  6. customseparated
  7. dry with materialdried over anhydrous magnesium sulphate
  8. customThe chloroform was removed by evaporation under reduced pressure
  9. customto leave an orange solid
  10. customThe solid was crystallised from toluene (1800 parts)

출처 및 근거

ORD 기록
ord-9e22dc87806148e682500f0b5c7f7d71
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05268490

연결된 노트

불러오는 중…