反応 #2467984

ord-bb1974f398bd452badbf5f9c40c8cd3f

反応方程式

COC(=O)C1CSCC1=O
4-oxo-3-methoxycarbonyltetrahydrothiophene
Cl.NO
hydroxylamine hydrochloride
COC(=O)c1cscc1N.Cl
title compound
収率 62.3%
COC(=O)c1cscc1N.Cl
Methyl 4-aminothiophene-3-carboxylate hydrochloride
収率 62.3%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 1 h
  2. 2
    温度The mixture was then cooled
  3. 3
    その他the solid which separated
  4. 4
    ろ過was filtered off
  5. 5
    洗浄washed with dry ether

実験手順

A mixture of 4-oxo-3-methoxycarbonyltetrahydrothiophene (6.5 g, 40.62 mmol), hydroxylamine hydrochloride (2.84 g, 40.62 mmol) and acetonitrile (30 mL) was stirred under reflux for 1 h. The mixture was then cooled and the solid which separated was filtered off and washed with dry ether to afford the title compound (4.9 g, 62%), mp 192-196° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08258119B2uspto-grants-2012_09