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

반응식

HRID 393663 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
50 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9924ef78b0284c45b6b40f18e00b8704
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06809097B1

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