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

HRID 1042775ノート

反応式

HRID 1042775 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
105 °C

実験手順

A mixture of Meldrum's acid (34.8 g, 0.42 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.

後処理

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

出典と根拠

ORDレコード
ord-fef88bf1ec624895ad0a438b6fbdd6e2
出典データセット
uspto-grants-2013_10
特許番号
US08557816B2

反応ノート

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