Chloral → HCID 86732907, compound

HRID 1579937Notes

Reaction equation

HRID 1579937 reaction equation
[O:1]=[CH:2][C:3]([Cl:6])([Cl:5])[Cl:4].[Cl-].[CH:8]([P+:11]([CH:20]([CH3:22])[CH3:21])([CH:17]([CH3:19])[CH3:18])OC=C(Cl)Cl)([CH3:10])[CH3:9]>CCOCC>[CH:8]([P:11]([CH:20]([CH3:22])[CH3:21])[CH:17]([CH3:19])[CH3:18])([CH3:10])[CH3:9].[O:1]=[CH:2][C:3]([Cl:6])([Cl:5])[Cl:4]

Participants

4

Reactant 2

HCID 6407ChloralHCID 86732908HCID 86732908, compound

Product 1

HCID 86732907HCID 86732907, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To chloral (200 ml.) heated to 60°C. under nitrogen was added 11.5 g. of triisopropyldichlorovinyloxyphosphonium chloride (from C-3 above). The clear solution was held overnight under nitrogen at 60°C. and then poured into 400 ml. of dry ether. The oil which first separated became crystalline on standing at room temperature. The solid was collected under nitrogen and recrystallized by dissolution in 80 ml. of dichloromethane and dilution with 400 ml. of dry ether. The crystalline 3/1 chloral/triisopropylphosphine reaction product was collected and dried under dry nitrogen.

Workup

  1. additionwas added 11.5 g
  2. additionpoured into 400 ml
  3. customThe oil which first separated
  4. customon standing at room temperature
  5. customThe solid was collected under nitrogen
  6. customrecrystallized by dissolution in 80 ml
  7. customThe crystalline 3/1 chloral/triisopropylphosphine reaction product
  8. customwas collected
  9. customdried under dry nitrogen

Sources & evidence

ORD record
ord-515c573686074f70b9df2d94a86feb93
Source dataset
uspto-grants-1976_01
Patent number
US03932318

Reaction notes

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