反応 #2045010

ord-85bd14b99fbc404f9f80ebedc96c78c6

反応方程式

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
収率 55.6%
Cl.Nc1ccc(OCCCCCC(=O)O)cc1
6-(4-Amino-phenoxy)-hexanoic acid Hydrochloride
収率 55.6%

反応条件

温度
10°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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