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

HRID 1195662노트

반응식

HRID 1195662 반응식
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

참가 물질

7

반응물 4

HCID 7914Diisopropyl EtherHCID 8030ThiopheneHCID 20479781Phenylmethyl 4-(2-chloro-2-oxoethyl)-1-piperidinecarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 31374Dimethylacetamide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-f0109f1715e245e9a194756130010a09
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112825

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