Dimethylamine → 1-[3,5-dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-2-yl)phenyl]-N,N-dimethylmethanamine

HRID 75229ノート

反応式

HRID 75229 の反応式
[CH3:1][NH:2][CH3:3].[H-].[Na+].[Cl:6][C:7]1[CH:12]=[C:11]([CH2:13]Cl)[CH:10]=[C:9]([Cl:15])[C:8]=1[C:16]1[NH:17][C:18]2[C:24]3[CH:25]=[CH:26][N:27]=[CH:28][C:23]=3[NH:22][C:21]3[N:29]=[CH:30][CH:31]=[CH:32][C:20]=3[C:19]=2[N:33]=1>CN(C)C=O.CO>[Cl:6][C:7]1[CH:12]=[C:11]([CH2:13][N:2]([CH3:3])[CH3:1])[CH:10]=[C:9]([Cl:15])[C:8]=1[C:16]1[NH:17][C:18]2[C:24]3[CH:25]=[CH:26][N:27]=[CH:28][C:23]=3[NH:22][C:21]3[N:29]=[CH:30][CH:31]=[CH:32][C:20]=3[C:19]=2[N:33]=1

参加物

6

反応物 3

HCID 674DimethylamineHCID 24758Sodium hydrideHCID 66887168HCID 66887168、化合物

生成物 1

HCID 160720251-[3,5-dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-2-yl)phenyl]-N,N-dimethylmethanamine収率 31%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

A solution of dimethylamine (23 μL, 2.0 M in tetrahydrofuran) was dissolved in N,N-dimethylformamide (0.5 mL) and cooled to 0° C. Sodium hydride (1.1 mg, 0.05 mmol) was added and the mixture was stirred for 15 minutes. 2-[2,6-dichloro-4-(chloromethyl)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4′,3′-f]azepine (10.0 mg, 0.02 mmol) was added and the mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with methanol and purified on preparative LCMS at pH 10 to give the desired product (3.2 mg, 31%). LC/MS: 437 (M+H)+.

後処理

  1. stirringthe mixture was stirred at room temperature for 16 hours
  2. custompurified on preparative LCMS at pH 10

出典と根拠

ORDレコード
ord-515c732e4eca48a186e7bf94a058eadd
出典データセット
uspto-grants-2014_09
特許番号
US08835423B2

反応ノート

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