Triethylamine → HCID 178514519、化合物

HRID 626741ノート

反応式

HRID 626741 の反応式
[N:1]([C:4]1[C:9]([F:10])=[CH:8][N:7]=[CH:6][C:5]=1[CH:11]=O)=[N+:2]=[N-:3].[Cl:13][C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([Cl:21])[C:15]=1[NH2:22].C(N(CC)CC)C>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[N:1]([C:4]1[C:9]([F:10])=[CH:8][N:7]=[CH:6][C:5]=1/[CH:11]=[N:22]/[C:15]1[C:14]([Cl:13])=[CH:19][C:18]([F:20])=[CH:17][C:16]=1[Cl:21])=[N+:2]=[N-:3]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 27740082,6-Dichloro-4-fluoroanilineHCID 866970534-Azido-5-fluoropyridine-3-carbaldehyde

生成物 1

HCID 178514519HCID 178514519、化合物

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a cooled (0° C.) solution of 4-azido-5-fluoro-pyridine-3-carbaldehyde (2.44 g, 14.7 mmol), 2,6-dichloro-4-fluorophenylamine (2.65 g, 14.7 mmol) and triethylamine (6.1 mL, 44 mmol) in DCM (50 mL) was added titanium tetrachloride (1M in DCM, 8.8 mL, 8.8 mmol) dropwise. The reaction mixture was stirred at 0° C. for 1 hour, warmed to room temperature, and stirred for a further 4 hours. The mixture was concentrated under reduced pressure. The residue was dissolved in toluene and filtered through Celite®. The filtrate was concentrated under to dryness under reduced pressure to afford the title compound that was used without further purification.

後処理

  1. temperaturewarmed to room temperature
  2. stirringstirred for a further 4 hours
  3. concentrationThe mixture was concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in toluene
  5. filtrationfiltered through Celite®
  6. concentrationThe filtrate was concentrated under to dryness under reduced pressure

出典と根拠

ORDレコード
ord-da6f08ddb3384eeab3f246e0db6b358c
出典データセット
uspto-grants-2016_04
特許番号
US09309240B2

反応ノート

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