Hydrazine, [4-[(trifluoromethyl)thio]phenyl]- → HCID 58731518, compound

HRID 500097

Reaction equation

HRID 500097 reaction equation
[F:1][C:2]([F:13])([F:12])[S:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10]N)=[CH:6][CH:5]=1.[CH3:14][CH:15]([C:24](=O)[CH3:25])[CH2:16][CH2:17][CH2:18][CH2:19][S:20]([OH:23])(=[O:22])=[O:21]>C(O)(=O)C>[F:1][C:2]([F:13])([F:12])[S:3][C:4]1[CH:9]=[C:8]2[C:7](=[CH:6][CH:5]=1)[N:10]=[C:24]([CH3:25])[C:15]2([CH3:14])[CH2:16][CH2:17][CH2:18][CH2:19][S:20]([OH:23])(=[O:21])=[O:22]

Participants

4

Reactant 2

HCID 10420564Hydrazine, [4-[(trifluoromethyl)thio]phenyl]-HCID 579033515-Methyl-6-oxoheptanesulfonic acid

Product 1

HCID 58731518HCID 58731518, compoundYield 14.2%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To 4-(trifluoromethylthio)phenylhydrazine (1 g) in acetic acid (40 ml) was added 5-methyl-6-oxoheptane-1-sulphonic acid (1.4 g) and the solution heated to reflux overnight. The volatiles were removed on a rotary evaporator to give the crude product, 1.1 g of which was purified by preparative HPLC. The relevant fractions were combined, concentrated on a rotary evaporator and freeze dried to give the desired product (260 mg). M+=381

Workup

  1. temperaturethe solution heated
  2. temperatureto reflux overnight
  3. customThe volatiles were removed on a rotary evaporator
  4. customto give the crude product, 1.1 g of which
  5. customwas purified by preparative HPLC
  6. concentrationconcentrated on a rotary evaporator and freeze
  7. customdried

Sources & evidence

ORD record
ord-7773518b75a34179bcb983a4bc6863e6
Source dataset
uspto-grants-2010_08
Patent number
US07767829B2

Linked notes

Loading…