Dimethylformamide → (4-[1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl}-phenyl)-acetic acid ethyl ester

HRID 472755ノート

反応式

HRID 472755 の反応式
[CH2:1]([O:3][C:4](=[O:24])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:21](=[O:22])[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[NH:14][C:13]2=[O:23])=[CH:8][CH:7]=1)[CH3:2].C([O-])([O-])=O.[K+].[K+].Br[CH2:32][C:33]([NH:35][C:36]1[CH:41]=[C:40]([Cl:42])[C:39]([O:43][CH3:44])=[CH:38][C:37]=1[O:45][CH3:46])=[O:34].CN(C=O)C>O>[CH2:1]([O:3][C:4](=[O:24])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:21](=[O:22])[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[N:14]([CH2:32][C:33](=[O:34])[NH:35][C:36]3[CH:41]=[C:40]([Cl:42])[C:39]([O:43][CH3:44])=[CH:38][C:37]=3[O:45][CH3:46])[C:13]2=[O:23])=[CH:8][CH:7]=1)[CH3:2]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 636790772-Bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamide2 回HCID 68589607[4-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-phenyl]-acetic acid ethyl ester2 回

生成物 1

HCID 68591686(4-[1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl}-phenyl)-acetic acid ethyl ester

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A round bottomed flask charged with [4-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-phenyl]-acetic acid ethyl ester (Intermediate H) (2.0 g, 6.17 mmol), K2CO3 (2.5 eq, 2.14 g, 15.52 mmol), and 2-bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamide (Intermediate C) (1.02 eq, 1.99 g, 6.49 mmol) is treated with dry DMF (20 ml). The reaction is stirred at RT for 72 hours. The reaction mixture is diluted with distilled water and stirred for 15 minutes. The precipitate formed was filtered, washed with water and dried under vacuum to give the title compound; [M+H]+ 552

後処理

  1. stirringstirred for 15 minutes
  2. customThe precipitate formed
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-3ac61f0de2454201a93cf62c879fe345
出典データセット
uspto-grants-2014_01
特許番号
US08633211B2

反応ノート

読み込み中…