Methylamine → HCID 44219587、化合物

HRID 452559

反応式

HRID 452559 の反応式
Br[CH2:2][C:3](=O)[CH:4]([C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=1)[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][CH:7]=1.[CH3:22][NH2:23].Br.C(S[C:28](=[NH:30])[NH2:29])C.[OH-].[Na+]>CO>[Br:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][CH:4]([C:3]2[N:30]=[C:28]([NH2:29])[N:23]([CH3:22])[CH:2]=2)[C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 6329MethylamineHCID 14798Sodium HydroxideHCID 200213S-Ethylisothiuronium bromideHCID 86650847HCID 86650847、化合物

生成物 1

HCID 44219587HCID 44219587、化合物収率 100.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

1-bromo-4-(4-bromophenyl)-3-(4-methoxyphenyl)butan-2-one (0.15 g, 0.36 mmol) was dissolved in methanol (1.8 mL) and methylamine (0.36 mL, 0.72 mmol, 2M solution in methanol) was added in one portion and the reaction was allowed to stir at 25° C. for 0.5 hour. S-ethylisothiourea hydrobromide (0.27 mg, 1.46 mmol) and NaOH (0.61 mL, 1.82 mmol, 3M solution in water) were added to the solution and the resulting solution was allowed to stir at 25° C. for 16 hours. The reaction was purified using reverse phase C-18 chromatography (acetontitrile and water system) to afford 140 mg of 4-[2-(4-bromophenyl)-1-(4-methoxyphenyl)ethyl]-1-methyl-1H-imidazol-2-amine as a yellow solid.

後処理

  1. stirringto stir at 25° C. for 16 hours
  2. customThe reaction was purified

出典と根拠

ORDレコード
ord-af88c8423c9e4317bb520879787aed68
出典データセット
uspto-grants-2013_07
特許番号
US08492387B2

関連ノート

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