Fuming sulfuric acid → HCID 12060806, compound

HRID 1728463Notes

Reaction equation

HRID 1728463 reaction equation
OS(O)(=O)=O.[O:6]=S(=O)=O.[Cl:10][C:11]([F:23])([C:19]([F:22])([F:21])[Cl:20])[C:12]([F:18])([F:17])[C:13](F)([F:15])I>>[Cl:10][C:11]([F:23])([C:19]([F:22])([F:21])[Cl:20])[C:12]([F:18])([F:17])[C:13]([F:15])=[O:6]

Participants

3

Reactant 2

HCID 24681Fuming sulfuric acid2×HCID 109269681,2-Dichloro-4-iodo-heptafluoro-N-butane

Product 1

HCID 12060806HCID 12060806, compound

Conditions

Temperature
110 °C

Procedure

A 1 L three-necked flask, fitted with a stir bar and condenser, was charged with 3.0 g of HgO (yellow), 125 mL of 20% oleum, 25 mL of 65% oleum and 75.6 g of 3,4-dichloro-1-iodoperfluorobutane. After the reaction mixture was heated at 110° C. for 2 hours, the condenser was replaced by a distillation head with a 250 mL flask for receiver cooled with ice water. Volatiles were collected, washed with 98% sulfuric acid to remove sulfur trioxide and redistilled to give 40.3 g of 3,4-dichloroperfluorobutyryl fluoride, bp 72°-75° C., 99.8% GC purity.

Workup

  1. customA 1 L three-necked flask, fitted with a stir bar and condenser
  2. customthe condenser was replaced by a distillation head with a 250 mL flask for receiver
  3. customVolatiles were collected
  4. washwashed with 98% sulfuric acid
  5. customto remove sulfur trioxide
  6. distillationredistilled

Sources & evidence

ORD record
ord-1fedb63226e94274a697c5683044c988
Source dataset
uspto-grants-1994_07
Patent number
US05326917

Reaction notes

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