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Pyridine → HCID 67283491, 화합물

HRID 1183154
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HRID 1183154 반응식
N1C=CC=CC=1.[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][CH:14]([NH2:16])[CH3:15])[CH:8]=1.[CH:17]1([CH3:29])[CH2:22][CH2:21][CH:20]([CH:23]([CH3:25])[CH3:24])[CH:19]([C:26](Cl)=[O:27])[CH2:18]1>O1CCCC1>[CH:23]([C@@H:20]1[CH2:21][CH2:22][C@@H:17]([CH3:29])[CH2:18][C@H:19]1[C:26]([NH:16][CH:14]([CH3:15])[CH2:13][C:9]1[CH:8]=[N:7][CH:12]=[CH:11][CH:10]=1)=[O:27])([CH3:25])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 47124581-(Pyridin-3-yl)propan-2-amineHCID 13734319Cyclohexanecarbonyl chloride, 5-methyl-2-(1-methylethyl)-

생성물 1

HCID 67283491HCID 67283491, 화합물수율 72.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 25 mL round bottom flask, fitted with magnetic stirrer, 15 mL of tetrahydrofuran, 1.5 mmol (1.5 eq.) of pyridine and 1.1 mmol (1.1 eq.) of 1-(pyridin-3-yl)propan-2-amine were added. p-Menthane carboxylic acid chloride (1.0 mmol) and the mixture was stirred at room temperature for 16 hours. The reaction mixture was extracted with MTBE and NaOH (1N in water). The organic layer was washed with brine, dried over MgSO4 and concentrated. The crude product was purified by column chromatography, obtaining 220 mg of a white solid, mp 108-110° C.

후처리

  1. customIn a 25 mL round bottom flask, fitted with magnetic stirrer
  2. extractionThe reaction mixture was extracted with MTBE and NaOH (1N in water)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-419ae74c17e9471e91839e5317539306
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08664261B2

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