Hydrochloric Acid → HCID 9856261, compound

HRID 1165298Notes

Reaction equation

HRID 1165298 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl[C:8]1([F:23])[C:12](Cl)([F:13])[O:11][C:10]([C:19]([F:22])([F:21])[F:20])([C:15]([F:18])([F:17])[F:16])[O:9]1.Cl.O1C=CCO1>O1CCCC1>[F:13][CH:12]1[CH:8]([F:23])[O:9][C:10]([C:15]([F:18])([F:16])[F:17])([C:19]([F:20])([F:21])[F:22])[O:11]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 1629194,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolaneHCID 21189139HCID 21189139, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 9856261HCID 9856261, compoundYield 69.1%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

In a round-bottomed flask was charged lithium aluminum hydride (3.8 g, 0.1 mole) in tetrahydrofuran (75 mL) and the contents was cooled in an ice-water bath at 0° to 5° C. 4,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (31.5 g, 0.1 mole) was added slowly. After the addition was complete, the reaction mixture was stirred at room temperature for 30 minutes. The resulting mixture was neutralized with 4.8N HCl (50 mL), then poured into 300 mL of ice-water. The bottom layer was separated and washed twice with cold water (200 mL). Distillation gave the saturated product 4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (17 g, 69% yield) instead of the unsaturated dioxole product.

Workup

  1. temperaturethe contents was cooled in an ice-water bath at 0° to 5° C
  2. additionAfter the addition
  3. customThe bottom layer was separated
  4. washwashed twice with cold water (200 mL)
  5. distillationDistillation

Sources & evidence

ORD record
ord-8c820ee835b64b77b9efe3c6f960c43c
Source dataset
uspto-grants-1990_03
Patent number
US04908461

Reaction notes

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