Реакция #630038

ord-ba7cb3b3a3a74618903faef23802b1b6

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was cooled with an external ice bath
  2. 2
    Температураwith cooling
  3. 3
    Концентрированиеconcentrated in vacuo
  4. 4
    ПромывкаThe methylene chloride solution was washed with water
  5. 5
    Сушкаa 5% sodium bicarbonate solution, water again, dried over sodium sulfate
  6. 6
    Другоеevaporated to dryness

Методика

One hundred grams of 1,2,3,4-tetrahydro-1-naphthol were dissolved in 1 liter of chloroform and 53.9 ml of pyridine. The mixture was cooled with an external ice bath and 98.6 ml of thionyl chloride were added over a 1 hour period. The reaction mixture was stirred an additional 2 hours with cooling, concentrated in vacuo, and the residue taken up in 1 liter of methylene chloride. The methylene chloride solution was washed with water, a 5% sodium bicarbonate solution, water again, dried over sodium sulfate, and evaporated to dryness to provide the desired intermediate 1,2,3,4-tetrahydro-1-chloronaphthalene.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04659730uspto-grants-1987_04