Cyclohexanone, 2-(hydroxymethylene)- → HCID 71253453、化合物

HRID 1029003

反応式

HRID 1029003 の反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].O[CH:12]=[C:13]1[CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=O>C(O)C>[Br:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:14]2[CH2:15][CH2:16][CH2:17][CH2:18][C:13]=2[CH:12]=[N:10]1

参加物

4

反応物 2

HCID 101871Cyclohexanone, 2-(hydroxymethylene)-HCID 27239122-Bromophenylhydrazine hydrochloride

生成物 1

HCID 71253453HCID 71253453、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Bromophenylhydrazine hydrochloride (1.00 g, 4.47 mmol) was added to a solution of 2-(hydroxymethylene)cyclohexanone (0.564 g, 4.47 mmol) in ethanol (20 mL) and the resulting solution was refluxed 3 h before being concentrated. The crude material was taken up in DCM and washed with saturated ammonium chloride, 1N NaOH, saturated sodium chloride, and dried over sodium sulfate. The solution was filtered and concentrated in vacuo to give 1-(2-bromophenyl)-4,5,6,7-tetrahydro-1H-indazole.

後処理

  1. temperaturethe resulting solution was refluxed 3 h
  2. concentrationbefore being concentrated
  3. washwashed with saturated ammonium chloride, 1N NaOH, saturated sodium chloride
  4. dry with materialdried over sodium sulfate
  5. filtrationThe solution was filtered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-533b0c10b45c4331af854929507f2e56
出典データセット
uspto-grants-2014_05
特許番号
US08735384B2

関連ノート

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