Hydrochloric Acid → HCID 178478946、化合物

HRID 419704ノート

反応式

HRID 419704 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([CH:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[NH:11][CH:12]=2)=[CH:4][C:3]=1[C:19]([F:22])([F:21])[F:20].[ClH:23]>CO>[ClH:23].[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([CH:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[NH:11][CH:12]=2)=[CH:4][C:3]=1[C:19]([F:20])([F:21])[F:22]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178505530HCID 178505530、化合物

生成物 1

HCID 178478946HCID 178478946、化合物収率 79%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Suspend 4-(4-(4-fluoro-3-(trifluoromethyl)phenyl)-1H-imidazol-2-yl)piperidine (250 mg, 0.80 mmol) in methanol (20 mL) and add hydrogen chloride (2 M in diethyl ether, 0.798 mL, 0.80 mmol). Stir at room temperature for 30 min. Concentrate the mixture in vacuo, and add water (15 mL) and acetonitrile (5 mL). Freeze-dry the mixture to afford an off-white solid. Dry the solid in vacuo at 100° C. for 2 h to afford 4-(4-(4-fluoro-3-(trifluoromethyl)phenyl)-1H-imidazol-2-yl)piperidine hydrochloride as an off-white solid (220 mg, 79%).

後処理

  1. concentrationConcentrate the mixture in vacuo
  2. additionadd water (15 mL) and acetonitrile (5 mL)
  3. customFreeze-dry the mixture
  4. customto afford an off-white solid
  5. customDry the solid in vacuo at 100° C. for 2 h

出典と根拠

ORDレコード
ord-f38627a8d60843368366e8c0ccddb51d
出典データセット
uspto-grants-2012_01
特許番号
US08093383B2

反応ノート

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