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

HRID 4375

反応式

HRID 4375 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-76b14a9408c64659932b886070897fcf
出典データセット
uspto-grants-1988_02
特許番号
US04725615

関連ノート

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