HCID 12298160, 화합물 → 4-Piperidinecarboxylic acid, 4-[(4-fluorophenyl)amino]-, methyl ester

HRID 1973807노트

반응식

HRID 1973807 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2([C:22]([O:24][CH3:25])=[O:23])[CH2:14][CH2:13][N:12](CC3C=CC=CC=3)[CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[H][H]>[Pd].CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2([C:22]([O:24][CH3:25])=[O:23])[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 12298160HCID 12298160, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 122981784-Piperidinecarboxylic acid, 4-[(4-fluorophenyl)amino]-, methyl ester

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 53 parts of methyl 4-[(4-fluorophenyl)amino]-1-(phenylmethyl)-4-piperidinecarboxylate and 400 parts of methanol is hydrogenated at normal pressure and at room temperature with 10 parts of palladium-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 15% of methanol, previously saturated with gaseous ammonia, as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue solidifies on scratching in hexane. The product is filtered off and dried, yielding methyl 4-[(4-fluorophenyl)amino]-4-piperidinecarboxylate; mp. 83.7° C.

후처리

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. customThe residue is purified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and 15% of methanol
  5. customThe pure fractions are collected
  6. customthe eluent is evaporated
  7. filtrationThe product is filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-58cb91c175e2425e847317b5fe557ca9
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998834

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