تفاعل #7721

ord-7db9ee3861144166bfa97d305c987b83

معادلة التفاعل

O=c1[nH]cnc2cc(F)ccc12
7-Fluoro-3H-quinazolin-4-one
Nc1cc(F)ccc1C(=O)O
2-amino-4-fluorobenzoic acid
CC(=O)O.N=CN
formamidine acetate
COCCO
2-methoxyethanol
NC(=O)Cn1cnc2cc(OCc3cccc(F)c3)ccc2c1=O
title compound
المردود 81.0%
NC(=O)Cn1cnc2cc(OCc3cccc(F)c3)ccc2c1=O
2-[7-(3-Fluoro-benzyloxy)-4-oxo-4H-quinazolin-3-yl]-acetamide
المردود 81.0%

المذيبات

ظروف التفاعل

درجة الحرارة
130°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    أخرىevaporated
  3. 3
    أخرىan off-white solid formed
  4. 4
    ترشيحthe solid filtered off
  5. 5
    غسيلwashed with water
  6. 6
    غسيلThe solid was then washed with hexane
  7. 7
    أخرىdried under high vacuum

الإجراء التجريبي

7-Fluoro-3H-quinazolin-4-one: A mixture of 2-amino-4-fluorobenzoic acid (14.6 g, 94 mmol) and formamidine acetate (19.6 g, 18.8 mmol) in 2-methoxyethanol (110 mL) was heated at 130° C. for 18 h. After cooling, the mixture was half evaporated and an off-white solid formed. The mixture was diluted with ammonia (25%, 10 mL in 90 mL water) and the solid filtered off and washed with water. The solid was then washed with hexane and dried under high vacuum to afford the title compound (12.5 g, 81%) as an off-white solid. MS: m/e=165.2 (M+H+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087612B2uspto-grants-2006_08