5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione → Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate

HRID 393663

反応式

HRID 393663 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH3:13])=[O:11])[NH2:6].[CH3:14][C:15]1([CH3:26])[O:20][C:19](=[O:21])[C:18](=[CH:22]OC)[C:17](=[O:25])[O:16]1>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH3:13])=[O:11])[NH:6][CH:22]=[C:18]1[C:17](=[O:25])[O:16][C:15]([CH3:14])([CH3:26])[O:20][C:19]1=[O:21]

参加物

4

反応物 2

HCID 1521115-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dioneHCID 168705Methyl 4-amino-o-anisate

生成物 1

HCID 22646557Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate収率 96.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
50 °C

実験手順

3-Methoxy-4-methoxycarbonylaniline (14.15 g, 78 mmol) was suspended in isopropanol and heated at 50° C. 2,2-Dimethyl-5-methoxymethylene-1,3-dioxane-4,6-dione (14.8 g, 80 mmol), (Montatsh. Chem. 1967, 98, 564), was then added in portions over 10 minutes and the mixture was heated at reflux for 30 minutes. The mixture was left to cool to ambient temperature overnight. The precipitate formed was collected by filtration, washed with isopropanol and dried under vacuum to give 5-((3-methoxy-4-methoxycarbonylanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (25.2 g, 96%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. waitThe mixture was left
  4. temperatureto cool to ambient temperature overnight
  5. customThe precipitate formed
  6. filtrationwas collected by filtration
  7. washwashed with isopropanol
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-9924ef78b0284c45b6b40f18e00b8704
出典データセット
uspto-grants-2004_10
特許番号
US06809097B1

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