Potassium Carbonate → HCID 54561569, 화합물

HRID 1683738노트

반응식

HRID 1683738 반응식
[CH:1](=[C:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C:9]1=[N:14][OH:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br.[CH2:17]([O:19][C:20]([C@@H:22]1[CH2:27][CH2:26][CH2:25][N:24]([CH2:28][CH2:29]Br)[CH2:23]1)=[O:21])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:17]([O:19][C:20]([C@@H:22]1[CH2:27][CH2:26][CH2:25][N:24]([CH2:28][CH2:29][O:15][N:14]=[C:9]2[CH2:10][CH2:11][CH2:12][CH2:13][C:8]2=[CH:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:23]1)=[O:21])[CH3:18]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 189199HCID 189199, 화합물HCID 70009171(R)-1-(2-bromoethyl)nipecotic acid ethyl ester hydrobromide

생성물 1

HCID 54561569HCID 54561569, 화합물수율 35.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of the above oxime (3.7 g, 18.4 mmol), (R)-1-(2-bromoethyl)-3-piperidinecarboxylic acid ethyl ester hydrobromide (7.0 g, 20.2 mmol, EP 374801), potassium carbonate (10.2 g, 73.5 mmol) and acetone (150 ml) was stirred at ambient temperature for 11 days. The mixture was filtered and the solvent evaporated in vacuo. The residue was purified by column chromatography on silica gel (200 g, heptane/ethyl acetate=3/2) to give 2.5 g of (R)-1-(2-(((2-(benzylidene)cyclohexylidene)amino)oxy)ethyl)-3-piperidinecarboxylic acid ethyl ester as an oil.

후처리

  1. filtrationThe mixture was filtered
  2. customthe solvent evaporated in vacuo
  3. customThe residue was purified by column chromatography on silica gel (200 g, heptane/ethyl acetate=3/2)

출처 및 근거

ORD 기록
ord-6a0a6e53df27443294320ae09860f0a5
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639766

반응 노트

불러오는 중…