تفاعل #49951

ord-4ace12a6e29447b3bbd6b021605bd28a

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe solid product was filtered
  2. 2
    غسيلwashed 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
    ترشيحthe solid product filtered
  8. 8
    أخرىair dried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424333uspto-grants-1995_06