反应 #2171075

ord-c86cfe3c25c0467797f05768a7a7033b

反应方程式

[K+].[OH-]
potassium hydroxide
C=[N+]=[N-]
diazomethane
C=[N+]=[N-]
diazomethane
O=C(O)c1cccc2oc3ccccc3c(=O)c12
9-Oxoxanthene-1-carboxylic acid
C=[N+]=[N-]
diazomethane
Cc1ccc(S(=O)(=O)N(C)N=O)cc1
N-methyl-N-nitrosotoluene-p-sulphonamide
COC(=O)c1cccc2oc3ccccc3c(=O)c12
ester
收率 100.0%
COC(=O)c1cccc2oc3ccccc3c(=O)c12
9-oxoxanthene-1-carboxylic acid methyl ester
收率 100.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他formed
  2. 2
    其他Removal of the solvent

实验过程

Esterification of acid can be achieved by several conventional methods by those skilled in the art. These procedures include utilizing diazomethane or methyl alcohol catalyzed by mineral acids. For example, ethereal diazomethane solution can be prepared for N-methyl-N-nitrosotoluene-p-sulphonamide and potassium hydroxide from a water bath. 9-Oxoxanthene-1-carboxylic acid (1.29 g, 5 mmol) in absolute methanol is added to this ethereal diazomethane solution at 0° C. until a pale yellow color formed. Removal of the solvent provides the desired ester solid in 100% yield. Thus the final products, Examples 5-9, can be prepared by condensation hydrazine with the ketonester 11 as described in General procedure C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716828B1uspto-grants-2004_04