Hydrochloric Acid → HCID 12786839, compound

HRID 2071Notes

Reaction equation

HRID 2071 reaction equation
[Cl:1][C:2]1(Cl)[CH2:5][C:4]([F:7])([F:6])[C:3]1([Cl:9])[F:8].O.Cl>CCOCC.C(N(CC)CC)C>[Cl:9][C:3]1([F:8])[C:2]([Cl:1])=[CH:5][C:4]1([F:7])[F:6]

Participants

6

Procedure

To a solution of 1,1,2 trichloro-2,3,3-trifluorocyclobutane (55.5 g) in 100 ml of anhydrous ether, triethylamine (40 ml) was added dropwise over 30 min at room temperature, and the mixture was stirred overnight at ambient temperature. The mixture was then stirred with 120 ml H2O and 7.5 ml of concentrated HCl. The ether layer was washed with H2O (100 ml), brine (100 ml), dried over anhydrous MgSO4, and evaporated in vacuo. The residue was distilled fractionally atmospheric pressure from 64°-68° C. to yield 36 g (79%) of a colorless liquid as pure product.

Workup

  1. washThe ether layer was washed with H2O (100 ml), brine (100 ml)
  2. dry with materialdried over anhydrous MgSO4
  3. customevaporated in vacuo
  4. distillationThe residue was distilled fractionally atmospheric pressure from 64°-68° C.

Sources & evidence

ORD record
ord-08d5189834b7446baa12a49af6278da7
Source dataset
uspto-grants-1998_03
Patent number
US05728694

Reaction notes

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