تفاعل #1135797

ord-dcc38955e6714627b69d85307b2d3c3a

معادلة التفاعل

COC(=O)Cl
methyl chloroformate
C1CCOC1
tetrahydrofuran
Cc1c(N)cccc1Cl
1-chloro-2-methyl-3-aminobenzene
COC(=O)Nc1cccc(Cl)c1C
1-chloro-2-methyl-3-methoxycarbonylaminobenzene

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىTo the reaction mixtures
  2. 2
    استخلاصthe resulting mixtures were extracted with ethyl acetate
  3. 3
    غسيلThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    تجفيفwere dried over anhydrous sodium sulfate
  5. 5
    تركيزThe mixtures were concentrated under reduced pressure

الإجراء التجريبي

Under cooling, to a mixture of methyl chloroformate 30 mL and tetrahydrofuran 50 mL was added dropwise 1-chloro-2-methyl-3-aminobenzene 5.00 g and the mixtures were stirred at 25° C. for a half hour. To the reaction mixtures was added water and the resulting mixtures were extracted with ethyl acetate. The organic layers were washed with aqueous saturated sodium bicarbonate solution and were dried over anhydrous sodium sulfate. The mixtures were concentrated under reduced pressure to give 1-chloro-2-methyl-3-methoxycarbonylaminobenzene 5.80 g.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09380782B2uspto-grants-2016_07