Chloride → HCID 20478459, compound

HRID 904678Notes

Reaction equation

HRID 904678 reaction equation
[CH2:1]([O:3][C:4]([C:6]1[O:24][C:10]2=[CH:11][CH:12]=[C:13]3[C:18]([N:17]=[C:16]([C:19]([O:21][CH3:22])=[O:20])[CH2:15][C:14]3=O)=[C:9]2[C:8](=[O:25])[CH:7]=1)=[O:5])[CH3:2].[Cl-:26].O>ClC(Cl)C>[CH2:1]([O:3][C:4]([C:6]1[O:24][C:10]2=[CH:11][CH:12]=[C:13]3[C:18]([N:17]=[C:16]([C:19]([O:21][CH3:22])=[O:20])[CH:15]=[C:14]3[Cl:26])=[C:9]2[C:8](=[O:25])[CH:7]=1)=[O:5])[CH3:2]

Participants

5

Reactant 3

HCID 312ChlorideHCID 962WaterHCID 131713238HCID 131713238, compound

Product 1

HCID 20478459HCID 20478459, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 63651,1-DichloroethaneSolvent

Procedure

The product of step (b) (1.3 g, 3.79 mmole) and phosporyl chloride (0.69 ml) in dry dichloroethane (80 ml) were heated to reflux for 15 minutes. The reaction mixture was then cooled and treated with water. The mixture was extracted with dichloroethane, the organic layer was washed with water, dried, and evaporated to give a brown solid. This was dried in vacuo over P2O5 at 50° C. to give the sub-title compound (0.9 g; 66%).

Workup

  1. temperatureto reflux for 15 minutes
  2. temperatureThe reaction mixture was then cooled
  3. extractionThe mixture was extracted with dichloroethane
  4. washthe organic layer was washed with water
  5. customdried
  6. customevaporated
  7. customto give a brown solid
  8. dry with materialThis was dried in vacuo over P2O5 at 50° C.

Sources & evidence

ORD record
ord-0841926e00f24ac0babe496b5e750910
Source dataset
uspto-grants-1983_12
Patent number
US04419352

Reaction notes

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