Ammonium Chloride → 5-(4-Methylpiperidin-1-yl)-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

HRID 1348551ノート

反応式

HRID 1348551 の反応式
Cl[C:2]1[N:7]2[CH:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([CH3:11])[C:3]=1[C:12]1[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:19].[CH3:20][CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.[Cl-].[NH4+]>C(Cl)(Cl)Cl>[CH3:20][CH:21]1[CH2:26][CH2:25][N:24]([C:2]2[N:7]3[CH:8]=[CH:9][N:10]=[C:6]3[N:5]=[C:4]([CH3:11])[C:3]=2[C:12]2[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:19])[CH2:23][CH2:22]1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 693814-MethylpiperidineHCID 230183375-Chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

生成物 1

HCID 230183085-(4-Methylpiperidin-1-yl)-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine収率 62.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

At room temperature, 45 mg (0.16 mmol) of 5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine and 63 mg (0.64 mmol) of 4-methylpiperidine were mixed. After one hour, chloroform and aqueous saturated ammonium chloride solution were added to the reaction mixture. The separated organic layer was washed with saturated brine, dried over sodium sulfate and concentrated. The residue was subjected to silica gel chromatography to give 35 mg (0.10 mmol, 61%) of 5-(4-methylpiperidin-1-yl)-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine.

後処理

  1. washThe separated organic layer was washed with saturated brine
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-35aa5fee19d247728c806d1d6912f90a
出典データセット
uspto-grants-2007_05
特許番号
US07211545B2

反応ノート

読み込み中…