Sodium Hydroxide → HCID 19063467, compound

Temperature

-5 °C

The ether XXVII was refractionated to obtain a sample (56.8 g, 0.286 mole) of <99% purity by GLC. This sample was cooled to -5°C and stirred in a teflon bottle as bromine trifluoride (15.6 g, 0.114 mole) was added dropwise. The product was stirred with ice and dilute sodium hydroxide solution to remove halogens and acids, separated, washed with distilled water, freeze-dried at -20°C and then dried at 0°C over type 3A molecular sieve. The V so obtained was 99.0% by GLC; micro b760 62.2°C; d42 1.41; yield 45 g (87% of theory). The molecular sieve type 3A is manufactured and sold by the Linde Division of Union Carbide Company.

1. customto obtain a sample (56.8 g, 0.286 mole) of <99% purity by GLC
2. additionwas added dropwise
3. customto remove halogens and acids
4. customseparated
5. washwashed with distilled water
6. customfreeze-dried at -20°C
7. dry with materialdried at 0°C over type 3A molecular sieve
8. customThe V so obtained
9. custommicro b760 62.2°C

ORD record

ord-6bd1a3a8350f454dad812ab9edeabe5d

Source dataset

uspto-grants-1976_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03943256