Sodium Carbonate → 2,4-Difluoro-5-iodobenzoic acid

2,4-Difluorobenzoic acid 10 (45.0 g, 285 mmol) was dissolved in concentrated sulfuric acid (360 mL) at 0° C. and N-iodosuccinimide (NIS, 64 g, 284 mmol) was added in portions at 0° C. The mixture was allowed to warm to room temperature (rt) and stirred 4 hours (h). The mixture was poured into ice water (approximately 1000 mL) and 10% aqueous sodium carbonate solution (80 mL) was added. After the mixture was stirred for 0.5 h, the precipitate was filtered, washed with water (approximately 2000 mL), then dried at 50° C. in a convection oven for 2 days to provide 76.3 g (94%) of 11 as a gray solid.

1. additionwas added
2. stirringAfter the mixture was stirred for 0.5 h
3. filtrationthe precipitate was filtered
4. washwashed with water (approximately 2000 mL)
5. customdried at 50° C. in a convection oven for 2 days

ORDレコード

ord-15bacb8cd0ea4af5b43b066be6af321f

出典データセット

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07994194B2