4-Aminopyridine → HCID 59427333, 화합물

HRID 1042845노트

반응식

HRID 1042845 반응식
[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[O:3]1.[CH:11](OCC)(OCC)OCC.[N:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][CH:22]=1>CCCCCC>[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[C:5](=[CH:11][NH:27][C:24]2[CH:25]=[CH:26][N:21]=[CH:22][CH:23]=2)[C:4](=[O:9])[O:3]1

참가 물질

5

반응물 3

HCID 17274-AminopyridineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformate

생성물 1

HCID 59427333HCID 59427333, 화합물

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
100 °C

실험 절차

In a dried 2-necked RBF equipped with reflux condenser and inert atmosphere, 2,2-dimethyl-1,3-dioxane-4,6-dione (2.33 g, 16 mmol) was dissolved in triethyl orthoformate (16 ml, 97 mmol) and the mixture was stirred at 100° C. under nitrogen for 1.5 h. On complete consumption of starting material (tic), pyridin-4-amine (1.5 g, 16 mmol) was added and heating continued for 4.5 h. The reaction mixture was cooled down to RT and poured into hexane (50 mL). The solid was filtered off and washed with hexane to afford 2,2-dimethyl-5-((pyridin-4-ylamino)methylene)-1,3-dioxane-4,6-dione as an orange solid.

후처리

  1. customIn a dried 2-necked RBF equipped
  2. temperaturewith reflux condenser
  3. additionwas added
  4. temperatureheating
  5. waitcontinued for 4.5 h
  6. temperatureThe reaction mixture was cooled down to RT
  7. filtrationThe solid was filtered off
  8. washwashed with hexane

출처 및 근거

ORD 기록
ord-1ee105765c84496b8ce91bfaa067f0c6
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557816B2

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