反应 #1122769

ord-6f989a21389d4c8b8420816143f6e655

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction is performed in a water/ice bath
  2. 2
    workup.STIRRINGThe reaction is stirred at 0° C. for 8 hours
  3. 3
    workup.WAITto stand at RT over night

实验过程

The reaction is performed in a water/ice bath. 500 mg (2.31 mmol, 1 eq) of 4-bromo-2-methoxy-6-methylaniline is dissolved in a mixture of 7 ml of acetic acid and 3 ml of water, followed by adding 0.8 ml of concentrated hydrochloric acid (37%) and 207 mg (3.00 mmol, 1.5 eq) of sodium nitrite dissolved in 1 ml of water. The mixture is stirred for 30 min and subsequently added to 8 ml of ice-cooled 50% by weight hypophosphoric acid. The reaction is stirred at 0° C. for 8 hours and allowed to stand at RT over night.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08546392B2uspto-grants-2013_10