p-Toluenesulfonic acid monohydrate → HCID 10018012、化合物

HRID 229728

反応式

HRID 229728 の反応式
[CH3:1][CH:2]1[CH2:11][C:10]2[NH:9][N:8]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)[CH2:6][C:5]=2[C:4](=[O:22])[CH2:3]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>N1C=CC=CC=1>[CH3:1][CH:2]1[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]=2[C:4](=[O:22])[CH2:3]1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 42467327-Methyl-3-(3-(trifluoromethyl)phenyl)-1,4,6,7,8-pentahydrocinnolin-5-one

生成物 1

HCID 10018012HCID 10018012、化合物収率 66.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a pyridine solution (1 mL) of 7-methyl-3-(3-trifluoromethylphenyl)-4,6,7,8-tetrahydro-1H-cinnolin-5-one (136.2 mg, 0.44 mmol) obtained in Example 65 was added p-toluenesulfonic acid hydrate (84 mg, 0.44 mmol) and stirred at room temperature for 3 days. The reaction liquid was concentrated, followed by purification of residue obtained with silica gel column chromatography (methylene chloride/methanol=30/1) to obtain an objective compound (89.0 mg, 66.1%).

後処理

  1. customThe reaction liquid
  2. concentrationwas concentrated
  3. customfollowed by purification of residue
  4. customobtained with silica gel column chromatography (methylene chloride/methanol=30/1)

出典と根拠

ORDレコード
ord-3d65f477759b46d29d8c9eeb51f701ee
出典データセット
uspto-grants-2009_07
特許番号
US07563893B2

関連ノート

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