Triethylamine → HCID 15336513, compound

HRID 1290828Notes

Reaction equation

HRID 1290828 reaction equation
C(N(CC)CC)C.[CH3:8][O:9][CH2:10][CH2:11][C:12]([N:14]([C:31](=[O:36])[C:32]([F:35])([F:34])[F:33])[C:15]1[C:20]([S:21](O)(=[O:23])=[O:22])=[CH:19][CH:18]=[CH:17][C:16]=1[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:13].P(Cl)(Cl)(Cl)(Cl)[Cl:38]>ClCCl>[CH3:8][O:9][CH2:10][CH2:11][C:12]([N:14]([C:31](=[O:36])[C:32]([F:35])([F:34])[F:33])[C:15]1[C:20]([S:21]([Cl:38])(=[O:23])=[O:22])=[CH:19][CH:18]=[CH:17][C:16]=1[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:13]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 24819Phosphorus pentachlorideHCID 15336512HCID 15336512, compound

Product 1

HCID 15336513HCID 15336513, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 3.8 g (7 mmol) of the N,N-diethylethanamine salt of 2-[(3-methoxy-1-oxopropyl)(trifluoroacetyl)amino][1,1'-biphenyl]-3-sulphonic acid in 14 ml of dichloromethane are added 1.75 g (8.4 mmol) of phosphorus pentachloride, the mixture is heated for 3 hours at the reflux temperature and is then concentrated under reduced pressure. The residue thus obtained is purified by chromatography on a column of silica gel, eluting with dichloromethane.

Workup

  1. temperaturethe mixture is heated for 3 hours at the reflux temperature
  2. concentrationis then concentrated under reduced pressure
  3. customThe residue thus obtained
  4. customis purified by chromatography on a column of silica gel
  5. washeluting with dichloromethane

Sources & evidence

ORD record
ord-1b4f881ceb6543f4b18a158dbe939612
Source dataset
uspto-grants-1998_05
Patent number
US05753667

Reaction notes

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