Hydrochloric Acid → 1-(2-Amino-4-fluorophenyl)piperidine-3-carboxamide hydrochloride

HRID 722233ノート

反応式

HRID 722233 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH2:11][CH:10]([C:14]([NH2:16])=[O:15])[CH2:9]2)=[C:4]([N+:17]([O-])=O)[CH:3]=1.[H][H].[ClH:22]>C1COCC1.C(OCC)(=O)C.[Pd]>[ClH:22].[NH2:17][C:4]1[CH:3]=[C:2]([F:1])[CH:7]=[CH:6][C:5]=1[N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14]([NH2:16])=[O:15])[CH2:9]1

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 218839121-(4-Fluoro-2-nitrophenyl)piperidine-3-carboxamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 218838991-(2-Amino-4-fluorophenyl)piperidine-3-carboxamide hydrochloride

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The solution of 2.67 g of 1-(4-fluoro-2-nitrophenyl)piperidine-3-carboxamide in 100 ml of THF was admixed with 260 mg of Pd/C. This mixture was hydrogenated in a shaking vessel at atmospheric pressure until the theoretical amount of hydrogen had been taken up. The mixture is then acidified with hydrogen chloride dissolved in ethyl acetate, the solid is filtered off with suction and washed with methanol, and the filtrate is concentrated under reduced pressure. The residue is triturated with tert-butyl methyl ether and the solid is filtered off with suction and dried under reduced pressure.

後処理

  1. filtrationthe solid is filtered off with suction
  2. washwashed with methanol
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe residue is triturated with tert-butyl methyl ether
  5. filtrationthe solid is filtered off with suction
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-460b37341dca48ddbd1f94fc12ac05d9
出典データセット
uspto-grants-2006_11
特許番号
US07138414B2

反応ノート

読み込み中…