反应 #155311

ord-18a1966deec047d38bc37b60ccbf4c99

反应方程式

CC1(C)OC(=O)CC(=O)O1
Meldrum's acid
COC([O-])[O-]
methyl orthoformate
CCCOc1cc2ccccc2cc1N
3-Propoxynaphthalen-2-ylamine
CCCOc1cc2ccccc2cc1NC=C1C(=O)OC(C)(C)OC1=O
2,2-dimethyl-5-[(3-propoxynaphthalen-2-ylamino) methylene][1,3]dioxane-4,6-dione
收率 95.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while heating
  2. 2
    温度under reflux
  3. 3
    workup.STIRRINGthe resulting mixture was stirred for 4 hours
  4. 4
    温度while heating
  5. 5
    温度under reflux
  6. 6
    浓缩concentrated to dryness under reduced pressure
  7. 7
    其他to recrystallize the residue from methanol

实验过程

Meldrum's acid (2.59 g, 17.9 mmol) was added to methyl orthoformate (16 ml), and the mixture was stirred for 2 hours while heating under reflux. 3-Propoxynaphthalen-2-ylamine (2.5 g, 12.4 mmol) was added thereto, and the resulting mixture was stirred for 4 hours while heating under reflux. The reaction mixture was cooled to room temperature and then concentrated to dryness under reduced pressure to recrystallize the residue from methanol, giving a pale brown powder of 2,2-dimethyl-5-[(3-propoxynaphthalen-2-ylamino) methylene][1,3]dioxane-4,6-dione (4.19 g, yield: 95%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE045108E1uspto-grants-2014_09