Bromotrichloromethane → HCID 9859700, compound

HRID 1455920Notes

Reaction equation

HRID 1455920 reaction equation
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.ClC(Cl)(Cl)Br.[S:25]1[CH:29]=[CH:28][CH:27]=[C:26]1[CH2:30][C:31]([OH:33])=O.[NH2:34][C:35]1[CH:40]=[C:39]([CH3:41])[CH:38]=[C:37]([CH3:42])[N:36]=1>O1CCCC1>[CH3:41][C:39]1[CH:38]=[C:37]([CH3:42])[N:36]=[C:35]([NH:34][C:31](=[O:33])[CH2:30][C:26]2[S:25][CH:29]=[CH:28][CH:27]=2)[CH:40]=1

Participants

6

Reactant 4

HCID 6383BromotrichloromethaneHCID 11776TriphenylphosphineHCID 159702-Thiopheneacetic acidHCID 215072-Amino-4,6-dimethylpyridine

Product 1

HCID 9859700HCID 9859700, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

9.22 g of triphenylphosphine, 6.93 ml of trichlorobromomethane, 5 g of 2-thienylacetic acid and 8.50 g of 2-amino-4,6-dimethylpyridine are dissolved in 120 ml of tetrahydrofuran. The mixture is brought to reflux and filtered, and the filtrate is concentrated; the residue is chromatographed on silica gel, eluting with dichloromethane, and the product obtained is recrystallized from isopropyl ether.

Workup

  1. temperatureto reflux
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated
  4. customthe residue is chromatographed on silica gel
  5. washeluting with dichloromethane
  6. customthe product obtained
  7. customis recrystallized from isopropyl ether

Sources & evidence

ORD record
ord-72666b6a4c1e41739536ea4e1ed4b23b
Source dataset
uspto-grants-1998_12
Patent number
US05843947

Reaction notes

Loading…