p-Toluenesulfonic acid monohydrate → HCID 136335902、化合物

HRID 2266447

反応式

HRID 2266447 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Cl:10][C:11]1[CH:24]=[CH:23][C:14]([CH2:15][CH:16]([C:20](=O)[CH3:21])[C:17](=O)[CH3:18])=[CH:13][CH:12]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.ClC1C=C(O)C=C2C=1C(C)=C(CC1C=CC(Cl)=CC=1)C(C)=N2>CO>[Cl:8][C:6]1[CH:5]=[C:4]([OH:9])[C:3]2[C:17]([CH3:18])=[C:16]([CH2:15][C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:24][CH:23]=3)[C:20]([CH3:21])=[N:1][C:2]=2[CH:7]=1

参加物

6

反応物 4

HCID 521998p-Toluenesulfonic acid monohydrateHCID 14888033-[(4-chlorophenyl)methyl]pentane-2,4-dioneHCID 199869473-Amino-5-chlorophenolHCID 136335922HCID 136335922、化合物

生成物 1

HCID 136335902HCID 136335902、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
160 °C

実験手順

A mixture of 3-amino-5-chlorophenol (0.46 g), 3-(4-chlorobenzyl)pentane-2,4-dione (0.72 g), and p-toluenesulfonic acid monohydrate (0.26 g) was heated at 160° C. for 2 hours. The mixture was cooled to room temperature, diluted with methanol (5.0 mL) and sonicated. The resulting precipitate was collected by filtration, washed with methanol and dried to afford a 50:50 mixture of title compound and 5-chloro-3-(4-chlorobenzyl)-2,4-dimethylquinolin-7-ol as an off-white solid, 0.67 g.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. customsonicated
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with methanol
  5. customdried
  6. customto afford

出典と根拠

ORDレコード
ord-2eda990c044447b0b2d27e0e8d3449e5
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

関連ノート

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