Dimethyl Sulfate → 6-Fluoro-1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one

HRID 4375

반응식

HRID 4375 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10]1[CH2:9][CH2:8][CH2:7][C:6](=[O:15])[C:5]2=1.[C:16](=O)([O-])[O-].[K+].[K+].COS(OC)(=O)=O>CC(C)=O>[F:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH3:16])[C:10]1[CH2:9][CH2:8][CH2:7][C:6](=[O:15])[C:5]2=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 3357046-fluoro-1,2,3,9-tetrahydro-4H-carbazol-4-one

생성물 1

HCID 201524556-Fluoro-1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one수율 97.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

후처리

  1. concentrationThe mixture was concentrated to one half of its volume
  2. filtrationThe mixture was filtered off
  3. washwashed with water (50 ml)
  4. customair-dried for 1 h
  5. dry with materialdried in vacuo over phosphorus pentoxide

출처 및 근거

ORD 기록
ord-76b14a9408c64659932b886070897fcf
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725615

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