2-Methylpropylenediamine → Benzonitrile, 4-[(2-amino-2-methylpropyl)amino]-

HRID 1259323ノート

反応式

HRID 1259323 の反応式
F[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[CH3:10][C:11]([NH2:15])([CH3:14])[CH2:12][NH2:13]>CO>[NH2:15][C:11]([CH3:14])([CH3:10])[CH2:12][NH:13][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 131282-MethylpropylenediamineHCID 145174-Fluorobenzonitrile

生成物 1

HCID 68731979Benzonitrile, 4-[(2-amino-2-methylpropyl)amino]-収率 88%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-Fluorobenzonitrile (7.0 g, 58 mmol) and 2-methylpropane-1,2-diamine (14 g, 160 mmol) were heated in a sealed vial in a microwave reactor (Biotage) at 180° C. for 25 minutes in two batches. Each batch was dissolved in methanol (50 mL) and then concentrated with silica to dryness. Flash chromatography on silica of each batch with neat acetonitrile and 2% triethylamine in acetonitrile as eluents gave 4-(2-amino-2-methylpropylamino)benzonitrile (9.58 g, 88% combined yield) as a white solid.

後処理

  1. concentrationconcentrated with silica to dryness

出典と根拠

ORDレコード
ord-0ba2b9d3241d4aa58a9a8c4131757a29
出典データセット
uspto-grants-2013_06
特許番号
US08466284B2

反応ノート

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