Acetic Acid → 6-Bromo-1,2,3,4-tetrahydrocarbazole

HRID 403646ノート

反応式

HRID 403646 の反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9]N)=[CH:5][CH:4]=1.[C:11](O)(=O)[CH3:12].C(=O)(O)[O-].[Na+]>C1(=O)CCCCC1>[Br:2][C:3]1[CH:8]=[C:7]2[C:6](=[CH:5][CH:4]=1)[NH:9][C:12]1[CH2:11][CH2:5][CH2:4][CH2:3][C:8]2=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 121574-Bromophenylhydrazine hydrochlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 2688776-Bromo-1,2,3,4-tetrahydrocarbazole

試薬・触媒・溶媒 1

HCID 7967Cyclohexanone溶媒2 回

実験手順

Cyclohexanone (1.16 mL, 11.2 mmol) and 4-bromo-phenylhydrazine hydrochloride (2.50 g, 11.2 mmol) were refluxed in cyclohexanone (18 mL) and acetic acid (AcOH) (12 L) for 24 h. The reaction mixture was treated with saturated sodium bicarbonate (Na2CO3) and extracted with ethyl acetate, dried (Na2CO3) and concentrated. The product was purified by column chromatography, giving 479 mg of compound 30 as a solid.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialdried (Na2CO3)
  3. concentrationconcentrated
  4. customThe product was purified by column chromatography

出典と根拠

ORDレコード
ord-cc728d06680b4570a0af222d9319c9df
出典データセット
uspto-grants-2014_06
特許番号
US08748451B2

反応ノート

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