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

HRID 1448289
ノート
印刷プレビュー

反応式

HRID 1448289 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-ec1e502f4af547adb76ccafd5b89513e
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04179569

反応ノート

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