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

HRID 1259323노트

반응식

HRID 1259323 반응식
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

참가 물질

4

반응물 2

HCID 131282-MethylpropylenediamineHCID 145174-Fluorobenzonitrile

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  1. concentrationconcentrated with silica to dryness

출처 및 근거

ORD 기록
ord-0ba2b9d3241d4aa58a9a8c4131757a29
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466284B2

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