Trimethyl orthoformate → 1,3-Dioxane-4,6-dione, 5-[[(6-methoxy-3-pyridinyl)amino]methylene]-2,2-dimethyl-

HRID 1013635노트

반응식

HRID 1013635 반응식
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[CH:11](OC)(OC)OC.[CH3:18][O:19][C:20]1[N:25]=[CH:24][C:23]([NH2:26])=[CH:22][CH:21]=1>CCCCCC>[CH3:18][O:19][C:20]1[N:25]=[CH:24][C:23]([NH:26][CH:11]=[C:6]2[C:7](=[O:8])[O:9][C:2]([CH3:10])([CH3:1])[O:3][C:4]2=[O:5])=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 9005Trimethyl orthoformateHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 811216-Methoxy-3-pyridinylamine

생성물 1

HCID 42557991,3-Dioxane-4,6-dione, 5-[[(6-methoxy-3-pyridinyl)amino]methylene]-2,2-dimethyl-

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
105 °C

실험 절차

A mixture of Meldrum's acid (34.8 g, 0.242 mol) and trimethyl orthoformate (285 mL, 2.05 mol) was heated to 105° C. for 2 h. To the solution 6-methoxypyridin-3-amine (30 g, 0.242 mol) was added and continued the stirring overnight at the same temperature. The mixture was allowed to cool to RT and diluted with hexane. The solid precipitated was filtered and washed with hexane to afford 5-((6-methoxypyridin-3-ylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione as a pale yellow solid.

후처리

  1. customthe stirring overnight
  2. temperatureto cool to RT
  3. customThe solid precipitated
  4. filtrationwas filtered
  5. washwashed with hexane

출처 및 근거

ORD 기록
ord-e2a3a80758684428b7001ed5c43d99d5
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981891B2

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