cis-1-[4-[3-Methoxy-4-[(phenylmethyl)amino]-1-piperidinyl]-1-oxobutyl]pyrrolidine → cis-1-[4-(4-Amino-3-methoxy-1-piperidinyl)-1-oxobutyl]pyrrolidine

HRID 1110389노트

반응식

HRID 1110389 반응식
[CH3:1][O:2][C@H:3]1[C@@H:8]([NH:9]CC2C=CC=CC=2)[CH2:7][CH2:6][N:5]([CH2:17][CH2:18][CH2:19][C:20]([N:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)=[O:21])[CH2:4]1.[H][H]>[Pd].CO>[NH2:9][C@H:8]1[CH2:7][CH2:6][N:5]([CH2:17][CH2:18][CH2:19][C:20]([N:22]2[CH2:23][CH2:24][CH2:25][CH2:26]2)=[O:21])[CH2:4][C@H:3]1[O:2][CH3:1]

참가 물질

5

반응물 2

HCID 70048899cis-1-[4-[3-Methoxy-4-[(phenylmethyl)amino]-1-piperidinyl]-1-oxobutyl]pyrrolidineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 70047197cis-1-[4-(4-Amino-3-methoxy-1-piperidinyl)-1-oxobutyl]pyrrolidine수율 71.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 53 parts of cis-1-[4-[3-methoxy-4-[(phenylmethyl)amino]-1-piperidinyl]-1-oxobutyl]pyrrolidine and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 3 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 28.3 parts (71.4%) of cis-1-[4-(4-amino-3-methoxy-1-piperidinyl)-1-oxobutyl]pyrrolidine as a residue (int. 43).

후처리

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-9a95bfd74b6f409daf8865967cb6ee72
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04975439

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