Ammonium Hydroxide → 3-Iodo-4-methylbenzamide

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (5.49 g, 28.6 mmol), 1H-benzo[d][1,2,3]triazol-1-ol hydrate (3.90 g, 28.9 mmol) and 32% aqueous ammonium hydroxide solution (1.10 mL, 28.7 mmol) were sequentially added to a stirred solution of 3-iodo-4-methylbenzoic acid (5.00 g, 19.1 mmol) in N,N′-dimethylformamide (15 mL) at room temperature. After stirring overnight, the mixture was concentrated in vacuo and water and dichloromethane were added to the mixture. The organic layer was washed with 2N aqueous sodium hydroxide solution, brine, dried (MgSO4) and evaporated to give the title compound (4.34 g, 70%) as a yellow solid.

1. concentrationthe mixture was concentrated in vacuo and water and dichloromethane
2. additionwere added to the mixture
3. washThe organic layer was washed with 2N aqueous sodium hydroxide solution, brine
4. dry with materialdried (MgSO4)
5. customevaporated

ORDレコード

ord-f45e531ea34f4ed4a834b05c1e81714b

出典データセット

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08772288B2