Dichloromethane → HCID 86601171, compound

HRID 1173327Notes

Reaction equation

HRID 1173327 reaction equation
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12](O)=[O:13])=[C:7]([O:15][CH3:16])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C(Cl)[Cl:18]>C(N(CC)CC)C>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([Cl:18])=[O:13])=[C:7]([O:15][CH3:16])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 6344DichloromethaneHCID 68717218HCID 68717218, compound

Product 1

HCID 86601171HCID 86601171, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

To 0.52 g (0.23 mmol) of the product of Step A was added 10 mL CH2Cl2 and 1 mL triethylamine. The resulting solution was concentrated in vacuo to remove the solvent and excess triethylamine. The residual triethylammonium salt was re-dissolved in 10 mL CH2Cl2 and 1.0 mL of oxalyl chloride was added. After stirring 30 min the reaction mixture was evaporated in vacuo to afford the title compound which was used in the next step without further purification.

Workup

  1. concentrationThe resulting solution was concentrated in vacuo
  2. customto remove the solvent and excess triethylamine
  3. dissolutionThe residual triethylammonium salt was re-dissolved in 10 mL CH2Cl2
  4. addition1.0 mL of oxalyl chloride was added
  5. customwas evaporated in vacuo

Sources & evidence

ORD record
ord-57d7b821f38544dc8b1aff73f6c34f07
Source dataset
uspto-grants-2010_11
Patent number
US07834062B2

Reaction notes

Loading…