Bromotrichloromethane → HCID 9859700, compound

HRID 727224Notes

Reaction equation

HRID 727224 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-66876d4a3f744680aeb52f7509694ccb
Source dataset
uspto-grants-1998_01
Patent number
US05712294

Reaction notes

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