Dichloromethane → 6-[2-[4-(2-Fluorophenoxymethyl)piperidino]ethyl]-1H-pyrazin-2-one

HRID 914892ノート

反応式

HRID 914892 の反応式
C([O:5][C:6]1[CH:11]=[N:10][CH:9]=[C:8]([CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][CH:17]([CH2:20][O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[F:28])[CH2:16][CH2:15]2)[N:7]=1)(C)(C)C.C(=O)([O-])[O-].[Na+].[Na+].ClCCl>C(OCC)(=O)C.Cl.C(OCC)(=O)C>[F:28][C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[O:21][CH2:20][CH:17]1[CH2:16][CH2:15][N:14]([CH2:13][CH2:12][C:8]2[NH:7][C:6](=[O:5])[CH:11]=[N:10][CH:9]=2)[CH2:19][CH2:18]1

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 222480162-Tert-butoxy 6-[2-[4-(2-fluorophenoxymethyl)piperidino]ethyl]pyrazine

生成物 1

HCID 97976346-[2-[4-(2-Fluorophenoxymethyl)piperidino]ethyl]-1H-pyrazin-2-one収率 79.1%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21866389Hydrogen chloride-ethyl acetate溶媒

実験手順

After dissolving 167 mg of 2-tert-butoxy 6-[2-[4-(2-fluorophenoxymethyl)piperidino]ethyl]pyrazine in 3 ml of ethyl acetate, 3 ml of 4N hydrogen chloride/ethyl acetate was added and the mixture was allowed to stand at room temperature for 30 minutes. Aqueous sodium carbonate solution was added to the reaction solution and extraction was performed with dichloromethane. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. Diethyl ether was added to the residue and the mixture was filtered to obtain the title compound (113 mg, 79% yield).

後処理

  1. additionwas added
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionDiethyl ether was added to the residue
  6. filtrationthe mixture was filtered

出典と根拠

ORDレコード
ord-fb047102c64a4ff1b7679e7ecb48df65
出典データセット
uspto-grants-2007_09
特許番号
US07265108B2

反応ノート

読み込み中…