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Thiophene → Ethyl cis-4-[(5-amino-4-chloro-2-methoxybenzoyl)amino]-3-methoxy-1-piperidinecarboxylate

HRID 981304
ノート
印刷プレビュー

反応式

HRID 981304 の反応式
[Cl:1][C:2]1[C:23]([N+:24]([O-])=O)=[CH:22][C:5]([C:6]([NH:8][C@H:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][C@H:10]2[O:20][CH3:21])=[O:7])=[C:4]([O:27][CH3:28])[CH:3]=1.S1C=CC=C1.[H][H]>CO.[Pt]>[NH2:24][C:23]1[C:2]([Cl:1])=[CH:3][C:4]([O:27][CH3:28])=[C:5]([CH:22]=1)[C:6]([NH:8][C@H:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][C@H:10]1[O:20][CH3:21])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8030ThiopheneHCID 67928767HCID 67928767、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 67928779Ethyl cis-4-[(5-amino-4-chloro-2-methoxybenzoyl)amino]-3-methoxy-1-piperidinecarboxylate収率 94%

試薬・触媒・溶媒 2

HCID 23939Platinum触媒
HCID 887
Methanol
溶媒
2 回

実験手順

A mixture of 90.5 parts of ethyl cis-4-[(4-chloro-2-methoxy-5-nitrobenzoyl)amino]-3-methoxy-1-piperidinecarboxylate, 3 parts of a solution of thiophene in methanol 4% and 400 parts of methanol was hydrogenated at normal pressure and at 50° C. with 5 parts of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 80 parts (94%) of ethyl cis-4-[(5-amino-4-chloro-2-methoxybenzoyl)amino]-3-methoxy-1-piperidinecarboxylate: mp. 142.5° C. (interm. 14).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was crystallized from 2-propanol
  4. filtrationThe product was filtered off
  5. customdried

出典と根拠

ORDレコード
ord-5a421704462c4aab8f8178eddca63923
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04990521

反応ノート

読み込み中…

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