Synthese du chloro-7 nitro-4 benzooxa-2 diazole-1,3 uniformement marque au carbone-14: Chlorure DE NBD-14C (U) “chloro - 4 nitro-7 benzofurazane 14C (U)”
✍ Scribed by Jean-Pierre Noel; Louis Pichat
- Publisher
- John Wiley and Sons
- Year
- 1977
- Tongue
- French
- Weight
- 444 KB
- Volume
- 13
- Category
- Article
- ISSN
- 0022-2135
No coin nor oath required. For personal study only.
✦ Synopsis
Abstract
The little compound, a useful reagent in biochemistry, has been synthasised in 14 steps from barium carbonate ^14^C via benzene ^14^C‐U, through aniline ^14^C‐U, p‐aminobenzene oulfamide ^14^C‐U and 2, 6 dichloroaniline ^14^ C(U). The axidation of the latter into 2,6 dichloronitrosobenzene ^14^ C(U) is best performed with m‐chloro peroxybenoic acid; other reagents reported in the literature give rise to substantial amounts of 2,6 dichloronitrobenzene ^14^ C‐U. Sodium axide and the 2,6 dichloronitrosobenzene ^14^ C(U) give p‐chlorobenzfurazane‐^14^ C(U). Nitration of the latter is conveniently obtained with the complex: trifluoromethan sulfonic acid + nitric acid which gives NBD, chloride ^14^ C(U) with a 96 % yield. The overall yield is 14% basen on Ba ^14^ CO~3~. Specific activity: 199 mci/mMoLe ‐ Schelf‐life at − 20°C, as liophilised power kept under vaccum, so for has been good.