反応 #2195522

ord-de3ae6ea0c2c4e8b81f91c4f3ae47a9c

反応方程式

CCCOC(=O)Cc1ccc(O)c(OC)c1
3-Methoxy-4-hydroxyphenylacetic acid propyl ester
CCCOC(=O)Cc1ccc(O)c(OC)c1
3-methoxy-4-hydroxyphenylacetic acid propyl ester
O=C([O-])[O-].[K+].[K+]
K2CO3
CCN(CC)C(=O)CCl
2-chloro-N,N-diethylacetamide
CCCOC(=O)Cc1ccc(OCC(=O)N(CC)CC)c(OC)c1
dark yellow oil
収率 95.0%
CCCOC(=O)Cc1ccc(OCC(=O)N(CC)CC)c(OC)c1
[4-[(N,N-diethylcarbamoyl)methoxyl]-3-methoxyphenyl]acetic acid propyl ester
収率 95.0%

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Under vigorous stirring, the suspension was warmed
  2. 2
    温度After cooling to room temperature the reaction mixture
  3. 3
    ろ過was filtered
  4. 4
    その他the remaining solvent removed under reduced pressure

実験手順

3-Methoxy-4-hydroxyphenylacetic acid propyl ester (15-A) was dissolved in acetone. To the solution, 2 equivalents of K2CO3 were added, followed by 1.2 equivalent of 2-chloro-N,N-diethylacetamide. Under vigorous stirring, the suspension was warmed to reflux (60° C.) for ˜15 hours. After cooling to room temperature the reaction mixture was filtered and the remaining solvent removed under reduced pressure, giving a 95% yield of a dark yellow oil. The oily product was purified by silica column chromatography to produce the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07514425B2uspto-grants-2009_04