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

HRID 1973807ノート

反応式

HRID 1973807 の反応式
[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

参加物

5

反応物 2

HCID 12298160HCID 12298160、化合物HCID 178418361HCID 178418361、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-58cb91c175e2425e847317b5fe557ca9
出典データセット
uspto-grants-1976_12
特許番号
US03998834

反応ノート

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