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Aluminum(III) Chloride → HCID 71730181、化合物

HRID 1487158
ノート
印刷プレビュー

反応式

HRID 1487158 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[F:5][C:6]1[CH:11]=[C:10]([I:12])[CH:9]=[CH:8][C:7]=1[NH:13][C:14]1[N:15]([CH3:48])[C:16](=[O:47])[C:17]([CH3:46])=[C:18]2[C:23]=1[C:22](=[O:24])[N:21](CC1C=CC(OC)=CC=1)[C:20](=[O:34])[N:19]2[C:35]1[CH:36]=[C:37]([CH2:41][CH2:42][C:43]([NH2:45])=[O:44])[CH:38]=[CH:39][CH:40]=1>C1(OC)C=CC=CC=1>[F:5][C:6]1[CH:11]=[C:10]([I:12])[CH:9]=[CH:8][C:7]=1[NH:13][C:14]1[N:15]([CH3:48])[C:16](=[O:47])[C:17]([CH3:46])=[C:18]2[C:23]=1[C:22](=[O:24])[NH:21][C:20](=[O:34])[N:19]2[C:35]1[CH:36]=[C:37]([CH2:41][CH2:42][C:43]([NH2:45])=[O:44])[CH:38]=[CH:39][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 898280783-(3-(5-((2-fluoro-4-iodophenyl)amino)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-3,4,6,7-tetrahydropyrido[4,3-d]pyrimidin-1(2H)-yl)phenyl) propanamide

生成物 1

HCID 71730181HCID 71730181、化合物収率 44%

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

Aluminium chloride (2.82 g, 21.14 mmol) was added in small portions to a solution of 3-(3-(5-((2-fluoro-4-iodophenyl)amino)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-3,4,6,7-tetrahydropyrido[4,3-d]pyrimidin-1(2H)-yl)phenyl)propanamide (1c) (1.500 g, 2.114 mmol) in anisole (15 ml). The resulting reaction mixture was stirred at room temperature for 24 h, then quenched by addition of MeOH (15 ml) and 2N HCl (0.5 ml). The resulting mixture was concentrated under vacuum and the residue thus obtained was purified by silica gel column chromatography to yield the titled compound (1) (0.450 g, 44%) [m/z=590.1 (M+1)].

後処理

  1. customThe resulting reaction mixture
  2. customquenched by addition of MeOH (15 ml) and 2N HCl (0.5 ml)
  3. concentrationThe resulting mixture was concentrated under vacuum
  4. customthe residue thus obtained
  5. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f599db0c2cff409b82070a71f788da54
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428499B2

反応ノート

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