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

HRID 274214

反応式

HRID 274214 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-ebc3585fa8d748dabc32d932e73856ec
出典データセット
uspto-grants-1995_02
特許番号
US05389597

関連ノート

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