Ethyl Acetate → 5-Chloro-1-(3-fluoro-5-methylbenzyl)-2-imino-1,2-dihydropyridine-3-carboxamide hydrobromide

HRID 1260880ノート

反応式

HRID 1260880 の反応式
[NH2:1][C:2]1[N:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].[Br:12][CH2:13][C:14]1[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([F:21])[CH:15]=1.C(OCC)(=O)C>CN(C=O)C>[BrH:12].[Cl:11][C:8]1[CH:7]=[C:3]([C:4]([NH2:6])=[O:5])[C:2](=[NH:1])[N:10]([CH2:13][C:14]2[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([F:21])[CH:15]=2)[CH:9]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 27784513-Fluoro-5-methylbenzyl bromideHCID 668768832-Amino-5-chloronicotinamide

生成物 1

HCID 686616225-Chloro-1-(3-fluoro-5-methylbenzyl)-2-imino-1,2-dihydropyridine-3-carboxamide hydrobromide収率 42.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-amino-5-chloronicotinamide (150 mg) and 1-(bromomethyl)-3-fluoro-5-methylbenzene (270 mg) in DMF (3 ml) was stirred at 100° C. for 24 hr. After cooling to room temperature, ethyl acetate was added, and the precipitated crystals were filtered and recrystallized to give the title compound (139 mg).

後処理

  1. filtrationthe precipitated crystals were filtered
  2. customrecrystallized

出典と根拠

ORDレコード
ord-eee8f1bdd6fe409ba3a510730a761f4d
出典データセット
uspto-grants-2013_06
特許番号
US08470859B2

反応ノート

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