Methanesulfonic Acid → HCID 86667998, compound

To a solution of product of step A (10.0 g, 33.4 mmol) in methanol (100 mL) at 0° C. was added potassium tert-butoxide (2.59 g, 23.1 mmol) portionwise and the mixture stirred for 40 min. The reaction mixture was concentrated in vacuo, and suspended in dichloromethane. To the suspension was added a solution of O-(mesitylsulfonyl)hydroxylamine (5.53 g, 33.4 mmol) in dichloromethane at 0° C. and the reaction stirred for 1 h. The mixture was then washed with cold 5% KOH solution and dried over anhydrous sodium sulfate. The organic layer was treated with methanesulfonic acid (1.75 mL, 26.72 mmol) then concentrated in vacuo to give crude O-(4-bromo-2-iodophenyl)hydroxylamine methanesulfonic acid salt (8.0 g, 58%) as a brown solid. CAUTION: This compound has potential to be shock sensitive and may be susceptible to decomposition. It should be handled with care and used directly without storage.

1. concentrationThe reaction mixture was concentrated in vacuo
2. stirringthe reaction stirred for 1 h
3. washThe mixture was then washed with cold 5% KOH solution
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationthen concentrated in vacuo

ORD record

ord-cd526939a6d844f7bb14c80c36901a02

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09067949B2