Реакция #49951

ord-4ace12a6e29447b3bbd6b021605bd28a

Уравнение реакции

CC(C)(C)NN.Cl
t-butyl hydrazine hydrochloride
Cc1ccccc1
toluene
O=C(Cl)C1C=c2ccc3cccc4ccc(c2c43)C1=O
pyrenonecarbonyl chloride
CCOCC
ether
CCCCCC
hexane
Cc1cccc(C(=O)N(NC(=O)C2C=c3ccc4cccc5ccc(c3c54)C2=O)C(C)(C)C)c1
N'-t-butyl-N-pyrenonecarbonyl-N'-(3-toluoyl)hydrazine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Фильтрацияthe solid product was filtered
  2. 2
    Промывкаwashed with water
  3. 3
    workup.STIRRINGThe solid product (0.5 g) was stirred in toluene (10 ml)
  4. 4
    workup.ADDITIONaqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise
  5. 5
    workup.STIRRINGAfter stirring for 5 hours
  6. 6
    workup.ADDITIONhexane and ether were added
  7. 7
    Фильтрацияthe solid product filtered
  8. 8
    Другоеair dried

Методика

To a stirred suspension of t-butyl hydrazine hydrochloride (0.02 mol) in toluene (20 ml) and aqueous hydroxide (5 ml of 50% solution) at room temperature was added pyrenonecarbonyl chloride (0.01 mol). After stirring the reaction mixture for 20 minutes, ether and hexane were added and the solid product was filtered and washed with water. The solid product (0.5 g) was stirred in toluene (10 ml) and aqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise. After stirring for 5 hours, hexane and ether were added and the solid product filtered and air dried.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05424333uspto-grants-1995_06