Chloroform → 4-(4-Ethylbenzyl)pyridazin-3-ol

HRID 2116508ノート

反応式

HRID 2116508 の反応式
[CH2:1]([C:3]1[CH:17]=[CH:16][C:6]([CH2:7][C:8]2[CH:13]=[CH:12][N:11]=[N:10][C:9]=2[O:14]C)=[CH:5][CH:4]=1)[CH3:2].C(Cl)(Cl)Cl>CO>[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:7][C:8]2[C:9](=[O:14])[NH:10][N:11]=[CH:12][CH:13]=2)=[CH:16][CH:17]=1)[CH3:2]

参加物

4

反応物 2

HCID 6212ChloroformHCID 23103618HCID 23103618、化合物

生成物 1

HCID 231036414-(4-Ethylbenzyl)pyridazin-3-ol収率 69%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

To a mixture of 4-(4-ethylbenzyl)-3-methoxy-pyridazine (2.11 g, 9.24 mmol) and chloroform (20 ml), trimethylsilyliodo (1.45 ml, 10.2 mmol) was added and this reaction mixture was stirred at 60° C. for 25 hours. After cooling to room temperature, the reaction mixture was diluted with methanol and concentrated. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to give the titled compound (1.36 g, 69%) as a yellow powder.

後処理

  1. additionwas added
  2. temperatureAfter cooling to room temperature
  3. concentrationconcentrated
  4. customThe resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1)

出典と根拠

ORDレコード
ord-c59ec7add83e48debea9ad6718e01f05
出典データセット
uspto-grants-2008_10
特許番号
US07439232B2

反応ノート

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