反応 #668815

ord-9af8614c6287478f9423faeb1aec397e

溶媒

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is cooled to 15-20° C.
  2. 2
    温度It is cooled to 10° C.
  3. 3
    workup.STIRRINGsubsequently stirred at 10° C. for 1 hour
  4. 4
    その他The product which is precipitated
  5. 5
    その他is isolated by filtration
  6. 6
    洗浄washed with water
  7. 7
    その他dried in vacuo at 800 C

実験手順

95.0 g of formic acid are added to 15.8 g of 1,8-diaminonaphthalene and the mixture is stirred at reflux temperature (100° C.) for 1 hour. Then 200 ml of water are added, and the mixture is cooled to 15-20° C. and adjusted to a pH of 8.5 by addition of 25% strength by weight ammonia. It is cooled to 10° C. and subsequently stirred at 10° C. for 1 hour. The product which is precipitated is isolated by filtration, washed with water and dried in vacuo at 800 C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05922086uspto-grants-1999_07