تفاعل #53350

ord-88e5633eab164bc19133f4639fe81750

معادلة التفاعل

CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C(=S)NN)OCO3
starting material XVIII
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C(=S)NN)OCO3
(±)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbothiohydrazide
CCOC(OCC)OCC
triethyl orthoformate
Cl
hydrochloric acid
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1c1nncs1)OCO3
title compound
المردود 77.0%
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1c1nncs1)OCO3
(±)-8-Methyl-5-(4-nitrophenyl)-7-(1,3,4-thiadiazol-2-yl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
المردود 77.0%

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling the precipitated crystals
  2. 2
    ترشيحwere filtered off
  3. 3
    غسيلwashed with ethanol
  4. 4
    أخرىdried

الإجراء التجريبي

A mixture of 0.57 g (1.43 mmol) of the starting material XVIII, 6 ml of triethyl orthoformate and a catalytic amount of hydrochloric acid was stirred at 80° C. for 1 h. After cooling the precipitated crystals were filtered off, washed with ethanol and dried to yield 0.45 g (77%) of the title compound; Mp.: 212-213° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858605B2uspto-grants-2005_02