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

HRID 722233노트

반응식

HRID 722233 반응식
[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

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 218839121-(4-Fluoro-2-nitrophenyl)piperidine-3-carboxamideHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-460b37341dca48ddbd1f94fc12ac05d9
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138414B2

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