Dichloromethane → 7-(3-hydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one

HRID 1162912ノート

反応式

HRID 1162912 の反応式
[Si]([O:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[CH:22]=[C:21]2[C:16]([CH:17]=[C:18]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]([F:33])([F:32])[F:31])[NH:19][C:20]2=[O:23])=[CH:15][CH:14]=1)(C(C)(C)C)(C)C.C(Cl)Cl>C1COCC1>[OH:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[CH:22]=[C:21]2[C:16]([CH:17]=[C:18]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]([F:33])([F:31])[F:32])[NH:19][C:20]2=[O:23])=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 6344DichloromethaneHCID 575581017-[3-(tert-butyldimethylsilyloxy)propylamino]-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one

生成物 1

HCID 231567767-(3-hydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one収率 101.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The 7-[3-(tert-butyldimethylsilyloxy)propylamino]-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (435 mg, 0.913 mmol) obtained in step A was dissolved in THF (9 ml). Thereafter, a 1 M tetrabutylammonium fluoride THF solution (1.1 ml, 1.1 mmol) was added to the obtained solution at a room temperature. The obtained mixture was stirred for 5 hours. Thereafter, methylene chloride was added to the reaction solution. An organic layer thereof was washed with a saturated saline solution, and was then dried over magnesium sulfate, followed by concentration under reduced pressure. The obtained residue was purified by silica gel chromatography (methylene chloride:methanol=30:1), so as to obtain 7-(3-hydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (337 mg, 95%).

後処理

  1. washAn organic layer thereof was washed with a saturated saline solution
  2. dry with materialwas then dried over magnesium sulfate
  3. concentrationfollowed by concentration under reduced pressure
  4. customThe obtained residue was purified by silica gel chromatography (methylene chloride:methanol=30:1)

出典と根拠

ORDレコード
ord-1fa931e1f50d42229998f1077252e940
出典データセット
uspto-grants-2010_10
特許番号
US07820693B2

反応ノート

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