Acetic Anhydride → 5-Acetyloxy-7-methyl-3-(3-trifluoromethylphenyl)-5,6,7,8-tetrahydrocinnoline

HRID 229719

反応式

HRID 229719 の反応式
[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[CH:4]([OH:22])[CH2:3]1.[C:23](OC(=O)C)(=[O:25])[CH3:24]>N1C=CC=CC=1>[C:23]([O:22][CH:4]1[CH2:3][CH:2]([CH3:1])[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]1=2)(=[O:25])[CH3:24]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 99725287-Methyl-3-(3-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydrocinnolin-5-ol

生成物 1

HCID 230867325-Acetyloxy-7-methyl-3-(3-trifluoromethylphenyl)-5,6,7,8-tetrahydrocinnoline収率 82.3%

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)-5,6,7,8-tetrahydrocinnolin-5-ol (61.6 mg, 0.2 mmol) obtained in Example 6 was added acetic anhydride (0.027 mL, 0.24 mmol) under ice cooling and subjected to reaction at room temperature for 2 hours. The reaction solution was concentrated as it is under reduced pressure, followed by purification of thus obtained residue using silica gel column chromatography (hexane/ethyl acetate=3/1) to obtain an objective compound (57.6 mg, 82.3%).

後処理

  1. customsubjected to reaction at room temperature for 2 hours
  2. concentrationThe reaction solution was concentrated as it
  3. customfollowed by purification of thus obtained residue

出典と根拠

ORDレコード
ord-189c5ebf90fb4674b2b639af22ac34f6
出典データセット
uspto-grants-2009_07
特許番号
US07563893B2

関連ノート

読み込み中…