1-(2,3-Dihydro-1H-indol-7-yl)ethan-1-one → 1-(1H-indol-7-yl)ethanone

HRID 4476

反応式

HRID 4476 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:12]=1[NH:11][CH2:10][CH2:9]2)(=[O:3])[CH3:2]>[O-2].[O-2].[Mn+4].C(Cl)Cl>[C:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:12]=1[NH:11][CH:10]=[CH:9]2)(=[O:3])[CH3:2]

参加物

4

反応物 1

HCID 136994211-(2,3-Dihydro-1H-indol-7-yl)ethan-1-one

生成物 1

HCID 137705341-(1H-indol-7-yl)ethanone収率 76%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒3 回HCID 6344Dichloromethane溶媒

実験手順

To 30 g. (0.186 mole) of 7-acetylindoline in 415 ml. of methylene chloride was added 48.5 g (0.56 mole) of manganese dioxide and the mixture refluxed through a soxhlet filled with 4A molecular sieves for 22 hours. The mixture was cooled and an additional 48.5 g. of manganese dioxide was added. Fresh molecular sieves were added and the refluxing continued for 5 hours. The same amount of manganese dioxide and molecular sieves were added again and the refluxing was continued for one hour. The mixture was filtered and the filtrate concentrated to dryness. The residue was triturated with hexane and filtered, 22.57 g. (76% yield), m.p. 65°-66° C.

後処理

  1. temperaturethe mixture refluxed through a soxhlet
  2. temperatureThe mixture was cooled
  3. additionFresh molecular sieves were added
  4. waitthe refluxing was continued for one hour
  5. filtrationThe mixture was filtered
  6. concentrationthe filtrate concentrated to dryness
  7. customThe residue was triturated with hexane
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-72e6c5070b794368854183d6caa959fa
出典データセット
uspto-grants-1988_02
特許番号
US04725616

関連ノート

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