Diisopropyl Ether → Benzyl 4-(2-oxoethyl)piperidine-1-carboxylate

HRID 1195662ノート

反応式

HRID 1195662 の反応式
Cl[C:2](=[O:20])[CH2:3][CH:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:11])[CH2:6][CH2:5]1.S1C=CC=C1.O(C(C)C)C(C)C.[H][H]>[Pd].CN(C)C(=O)C>[O:20]=[CH:2][CH2:3][CH:4]1[CH2:5][CH2:6][N:7]([C:10]([O:12][CH2:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[O:11])[CH2:8][CH2:9]1

参加物

7

反応物 4

HCID 7914Diisopropyl EtherHCID 8030ThiopheneHCID 20479781Phenylmethyl 4-(2-chloro-2-oxoethyl)-1-piperidinecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22278282Benzyl 4-(2-oxoethyl)piperidine-1-carboxylate収率 95.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 31374Dimethylacetamide溶媒

実験手順

A mixture of 90 parts of (phenylmethyl) 4-(2- chloro-2-oxoethyl)-1-piperidinecarboxylate, 90 parts of N,N-dimethylacetamide 6 parts of a thiophene solution and 438 parts of 2,2'-oxybispropane was hydrogenated at normal pressure and at room temperature in the presence of 5 parts of palladium-on-charcoal 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was taken up in water. The separated organic layer was dried, filtered and evaporated, yielding 75 parts (95.7%) of (phenylmethyl) 4-(2-oxoethyl)-1-piperidinecarboxylate as a residue (interm. 7).

後処理

  1. filtrationthe catalyst was filtered off
  2. customThe separated organic layer was dried
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-f0109f1715e245e9a194756130010a09
出典データセット
uspto-grants-1992_05
特許番号
US05112825

反応ノート

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