Triethylamine → 5-Bromo-3-(4-(4-methylpiperazin-1-yl)phenylamino)picolinonitrile

HRID 535903ノート

反応式

HRID 535903 の反応式
[Br:1][C:2]1[CH:3]=[C:4](F)[C:5]([C:8]#[N:9])=[N:6][CH:7]=1.[CH3:11][N:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=2)[CH2:14][CH2:13]1.C(N(CC)CC)C>C(O)(C)C>[Br:1][C:2]1[CH:3]=[C:4]([NH:22][C:21]2[CH:20]=[CH:19][C:18]([N:15]3[CH2:14][CH2:13][N:12]([CH3:11])[CH2:17][CH2:16]3)=[CH:24][CH:23]=2)[C:5]([C:8]#[N:9])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 7372534-(4-Methylpiperazin-1-yl)anilineHCID 441966805-Bromo-3-fluoropyridine-2-carbonitrile

生成物 1

HCID 704984275-Bromo-3-(4-(4-methylpiperazin-1-yl)phenylamino)picolinonitrile

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A solution of 5-bromo-3-fluoropicolinonitrile (1 g, 5 mmol), from EXAMPLE 49A, and 4-(4-methylpiperazin-1-yl)aniline (1.24 g, 6.5 mmol) in isopropanol (15 mL) was treated with triethylamine (0.76 mL, 7.5 mmol) was subjected to microwave irradiation (Biotage, Initiator) at 180° C. for 2 hours. The reaction mixture was concentrated and purified on silica gel with 2-25% methanol in dichloromethane to afford the title compound.

後処理

  1. customwas subjected to microwave irradiation (Biotage, Initiator) at 180° C. for 2 hours
  2. concentrationThe reaction mixture was concentrated
  3. custompurified on silica gel with 2-25% methanol in dichloromethane

出典と根拠

ORDレコード
ord-df63f681c736471b955f6d432f0e4ef0
出典データセット
uspto-grants-2014_10
特許番号
US08859546B2

反応ノート

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