Ethyl Acetate → 2,3-Dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

HRID 61863

反応式

HRID 61863 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][C:14]=1[Cl:15])[NH:11][C:10]1[C:9]([CH3:17])([CH3:16])[C:8]3[CH:18]=[C:19]([O:22]C)[CH:20]=[CH:21][C:7]=3[C:6](=[O:24])[C:5]2=1.[Cl-].[NH+]1C=CC=CC=1.C(OCC)(=O)C>O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][C:14]=1[Cl:15])[NH:11][C:10]1[C:9]([CH3:17])([CH3:16])[C:8]3[CH:18]=[C:19]([OH:22])[CH:20]=[CH:21][C:7]=3[C:6](=[O:24])[C:5]2=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 69401Einecs 211-027-4HCID 668343702,3-Dichloro-8-methoxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

生成物 1

HCID 668345622,3-Dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

Mixture of 2,3-dichloro-8-methoxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound Y3, 16.5 mg, 0.0457 mmol) and pyridinium chloride (0.2 g) was stirred at ambient temperature of 160° C. for 7 hr. The reaction mixture was cooled to room temperature and added with ethyl acetate and water. The mixture was extracted three times with ethyl acetate. The organic layer was washed twice with water, dried over sodium sulfate, and concentrated under reduced pressure. The resulting crude product was used for the next step without further purification (brown solid, 14.8 mg, 94%).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washThe organic layer was washed twice with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting crude product was used for the next step without further purification (brown solid, 14.8 mg, 94%)

出典と根拠

ORDレコード
ord-c23d8becc1b5464fac70565077e5f0e9
出典データセット
uspto-grants-2016_09
特許番号
US09440922B2

関連ノート

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