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Ammonium Hydroxide → Phenylamino-1-(2-phenylethyl)-4-piperidinecarboxylic acid

HRID 1973791
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HRID 1973791 반응식
C1(N[C:8]2([C:22]([O:24]CC3C=CC=CC=3)=[O:23])[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:10][CH2:9]2)C=CC=CC=1.[OH-].[NH4+:33]>[Pd].CO>[C:16]1([NH:33][CH:10]2[CH2:9][CH:8]([C:22]([OH:24])=[O:23])[CH2:13][CH2:12][N:11]2[CH2:14][CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 12298150Phenylmethyl 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylate

생성물 1

HCID 86734310Phenylamino-1-(2-phenylethyl)-4-piperidinecarboxylic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 60 parts of phenylmethyl 4-(phenylamino)-1-(2-phenylethyl)-4-piperidinecarboxylate and 320 parts of methanol is hydrogenated at normal pressure and at room temperature with 10 parts of palladium-on-charcoal catalyst 10%. Upon the addition of a concentrated ammonium hydroxide solution, the precipitate, which is formed during the hydrogenation, is dissolved. The catalyst is filtered off and the filtrate is concentrated. Methanol is added and the whole is concentrated again. After cooling to room temperature the product is filtered off and dried in vacuo at 120° C, yielding 43.7 parts of 4-(phenylamino-1-(2-phenylethyl)-4-piperidinecarboxylic acid; mp. 268° C.

후처리

  1. customthe precipitate, which is formed during the hydrogenation
  2. dissolutionis dissolved
  3. filtrationThe catalyst is filtered off
  4. concentrationthe filtrate is concentrated
  5. additionMethanol is added
  6. concentrationthe whole is concentrated again
  7. filtrationis filtered off
  8. customdried in vacuo at 120° C

출처 및 근거

ORD 기록
ord-c6692313b7da4e0aa778971ac01cf6cb
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03998834

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