反应 #2045010

ord-85bd14b99fbc404f9f80ebedc96c78c6

反应方程式

COC(=O)CCCCCOc1ccc(NC(C)=O)cc1
6-(4-Acetylaminophenoxy)hexanoic acid methyl ester
COC(=O)CCCCCOc1ccc(NC(C)=O)cc1
6-(4-Acetylamino-phenoxy)-hexanoic acid methyl ester
Cl
hydrochloric acid
Cl.Nc1ccc(OCCCCCC(=O)O)cc1
20
收率 55.6%
Cl.Nc1ccc(OCCCCCC(=O)O)cc1
6-(4-Amino-phenoxy)-hexanoic acid Hydrochloride
收率 55.6%

反应条件

温度
10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 48 hours
  2. 2
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled off in vacuum
  3. 3
    过滤filtered hot
  4. 4
    过滤filtered
  5. 5
    其他dried

实验过程

A mixture of 6-(4-Acetylaminophenoxy)hexanoic acid methyl ester 19 (290 grams, 1.04 mol) in concentrated hydrochloric acid (7.12 L) was refluxed for 48 hours. Excess concentrated hydrochloric acid was distilled off in vacuum and filtered hot. The mixture was cooled to 10° C., filtered and dried give pure 20 (150 g, 55.6%) as a brown powder. The melting point was found to be 155-160° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08409559B2uspto-grants-2013_04