Triethylamine → N,N-Dimethyl-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridin-2-amine

HRID 627489ノート

反応式

HRID 627489 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=2)=[O:9])=[CH:4][N:3]=1.Cl.[CH3:17][NH:18][CH3:19].CCN(CC)CC>CO>[CH3:17][N:18]([CH3:19])[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=2)=[O:9])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 120166732-Chloro-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridine2 回

生成物 1

HCID 86716071N,N-Dimethyl-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridin-2-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
75 °C

実験手順

In a 50-mL round-bottom flask was placed a solution of 2-chloro-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridine (250 mg, 1.13 mmol, Intermediate 22, step c), dimethylamine hydrochloride (96 mg, 1.2 mmol), and Et3N (342 mg, 3.39 mmol) in methanol (15 mL). The resulting mixture was heated at 75° C. overnight and concentrated under vacuum. The residue was purified by flash column chromatography (silica gel column, 100:0-20:1 CH2Cl2/MeOH) to give the title compound as a light yellow solid.

後処理

  1. customIn a 50-mL round-bottom flask was placed
  2. concentrationconcentrated under vacuum
  3. customThe residue was purified by flash column chromatography (silica gel column, 100:0-20:1 CH2Cl2/MeOH)

出典と根拠

ORDレコード
ord-e7ec708e8e7440d5af384e792da973a2
出典データセット
uspto-grants-2016_04
特許番号
US09309222B2

反応ノート

読み込み中…