5-cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid → 2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-5-carbonitrile

HRID 2401174ノート

反応式

HRID 2401174 の反応式
[C:1]([C:3]1[CH:4]=[C:5]2[C:11](C(O)=O)=[C:10]([C:15]([F:18])([F:17])[F:16])[NH:9][C:6]2=[N:7][CH:8]=1)#[N:2]>O.CN1CCCC1=O>[F:18][C:15]([F:16])([F:17])[C:10]1[NH:9][C:6]2=[N:7][CH:8]=[C:3]([C:1]#[N:2])[CH:4]=[C:5]2[CH:11]=1

参加物

4

反応物 1

HCID 671123375-cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid2 回

生成物 1

HCID 671115072-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-5-carbonitrile収率 61.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
120 °C

実験手順

5-Cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid (Intermediate 3, 2.49 g, 9.76 mmol) was dissolved in water (36 mL) and N-methyl-2-pyrrolidone (48 mL). The resulting mixture was heated at 120° C. for 18 hours. The reaction mixture was allowed to cool to room temperature and diluted with water. The resulting precipitate was collected by filtration, washed with water and dried under high vacuum at 40° C. for 5 hours to give the title compound as a white solid (1.26 g);

後処理

  1. temperatureto cool to room temperature
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried under high vacuum at 40° C. for 5 hours

出典と根拠

ORDレコード
ord-2f28891b36df4361b27dfb5b76c5c03b
出典データセット
uspto-grants-2014_08
特許番号
US08796283B2

反応ノート

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