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

HRID 414415

반응식

HRID 414415 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매3회HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2987f06fb0a04cb8b72d55deb7bbf38b
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04791129

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