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Water → 6-(azepan-4-yloxy)-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one

HRID 2059589
ノート
印刷プレビュー

反応式

HRID 2059589 の反応式
[NH:1]1[CH2:7][CH2:6][CH2:5][CH:4]([OH:8])[CH2:3][CH2:2]1.[H-].[Na+].F[C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][C:21]=1[CH3:22])[C:18](=[O:23])[N:17]([CH2:24][C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1)[CH:16]=[CH:15]2.O>CC(N(C)C)=O>[NH:1]1[CH2:7][CH2:6][CH2:5][CH:4]([O:8][C:12]2[CH:13]=[C:14]3[C:19](=[CH:20][C:21]=2[CH3:22])[C:18](=[O:23])[N:17]([CH2:24][C:25]2[CH:26]=[CH:27][C:28]([O:31][CH3:32])=[CH:29][CH:30]=2)[CH:16]=[CH:15]3)[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydride2 回HCID 5149746Azepan-4-ol2 回HCID 592260436-fluoro-2-(4-methoxybenzyl)-7-methylisoquinolin-1(2H)-one2 回

生成物 1

HCID 685558126-(azepan-4-yloxy)-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one収率 41%

試薬・触媒・溶媒 1

HCID 31374
Dimethylacetamide
溶媒
2 回

実験手順

A solution of 58 mg (0.51 mmol) azepan-4-ol in 5 ml dimethylacetamide was stirred with 45 mg (1.52 mmol) 80 percent sodium hydride for 45 minutes at room temperature. Then 150 mg (0.51 mmol) 6-fluoro-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one in dimethylacetamide was added. The reaction mixture was heated to 80° C. for 3 days during which additional amounts of azepan-4-ol and sodium hydride were added until complete conversion of the 6-fluoro-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one was obtained. The reaction mixture was slowly added to 10 ml water and after 1 h of stirring the product was isolated by filtration and dried overnight in vacuum. 82 mg of 6-(azepan-4-yloxy)-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one were obtained.

後処理

  1. customwas obtained
  2. customwas isolated by filtration
  3. customdried overnight in vacuum

出典と根拠

ORDレコード
ord-e58dfde0a0374274af02074f24a4e936
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08278294B2

反応ノート

読み込み中…

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