反応 #348072

ord-222415fb05e64196981cfd7fb30e071f

溶媒

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is cooled to 80° C.
  2. 2
    温度the mixture is cooled to room temperature
  3. 3
    ろ過filtered with suction
  4. 4
    洗浄After the residue has been washed with 240 ml of methanol
  5. 5
    その他dried at 150° C.
  6. 6
    その他88.8 g of the stated dyestuff are obtained in a very good quality

実験手順

250 g of phenol are melted at about 60° C. 47.4 g of 1,8-diaminonaphthalene and 59.4 g of 1,8-naphthalic acid anhydride are introduced, while passing over nitrogen, and the mixture is heated to 150° C. in the course of 1 hour and kept at this temperature for 2 hours. The reaction mixture is cooled to 80° C., 120 ml of methanol are added at a temperature of 80° to 65° C. in the course of 30 minutes, and the mixture is cooled to room temperature and filtered with suction. After the residue has been washed with 240 ml of methanol and dried at 150° C., 88.8 g of the stated dyestuff are obtained in a very good quality.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05530130uspto-grants-1996_06