Hydrochloric Acid → N-(3-(1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-(imidazo[1,2-a]pyrazin-3-ylethynyl)-4-methylbenzamide mono hydrochloride salt

HRID 923191ノート

反応式

HRID 923191 の反応式
[N:1]1([C:6]2[CH:7]=[C:8]([NH:16][C:17](=[O:36])[C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[C:20]([C:25]#[C:26][C:27]4[N:31]5[CH:32]=[CH:33][N:34]=[CH:35][C:30]5=[N:29][CH:28]=4)[CH:19]=3)[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[ClH:37]>CC#N>[ClH:37].[N:1]1([C:6]2[CH:7]=[C:8]([NH:16][C:17](=[O:36])[C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[C:20]([C:25]#[C:26][C:27]4[N:31]5[CH:32]=[CH:33][N:34]=[CH:35][C:30]5=[N:29][CH:28]=4)[CH:19]=3)[CH:9]=[C:10]([C:12]([F:15])([F:13])[F:14])[CH:11]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 16214860N-(3-(1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-(imidazo[1,2-a]pyrazin-3-ylethynyl)-4-methylbenzamide

生成物 1

HCID 86614280N-(3-(1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-(imidazo[1,2-a]pyrazin-3-ylethynyl)-4-methylbenzamide mono hydrochloride salt

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
50 °C

実験手順

N-(3-(1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-(imidazo[1,2-a]pyrazin-3-ylethynyl)-4-methylbenzamide (0.94 mmol) can be suspended in MeCN (10 ml) and heated with stirring to a temperature of 45 to 55° C. (hot plate temperature). Hydrochloric acid (1.1 eq 1M solution in EtOH) is added to obtain dissolution. Within a few minutes, a precipitate is allowed to form. The suspension can be cooled to ambient temperature and then filtered and washed with MeCN (1×1.5 ml liquors+1×1.5 ml fresh). The solid can be dried at 50° C. under vacuum to constant weight.

後処理

  1. temperatureheated
  2. customto obtain
  3. dissolutiondissolution
  4. waitWithin a few minutes
  5. customto form
  6. temperatureThe suspension can be cooled to ambient temperature
  7. filtrationfiltered
  8. washwashed with MeCN (1×1.5 ml liquors+1×1.5 ml fresh)
  9. customThe solid can be dried at 50° C. under vacuum to constant weight

出典と根拠

ORDレコード
ord-b8968f9d5cde4009993bda4c32c704b3
出典データセット
uspto-grants-2016_03
特許番号
US09278971B2

反応ノート

読み込み中…