Hydrochloric Acid → HCID 22763213, compound

HRID 1112764Notes

Reaction equation

HRID 1112764 reaction equation
[C:1]1(=[O:10])[O:9][C:6]([CH3:8])([CH3:7])[O:5][C:3](=[O:4])[CH2:2]1.C(N(CC)CC)C.[F:18][C:19]([F:30])([F:29])[C:20]1[CH:25]=[CH:24][C:23]([N:26]=[C:27]=[O:28])=[CH:22][CH:21]=1.Cl>CS(C)=O.O>[CH3:7][C:6]1([CH3:8])[O:9][C:1](=[O:10])[C:2]([C:27](=[O:28])[NH:26][C:23]2[CH:24]=[CH:25][C:20]([C:19]([F:18])([F:30])[F:29])=[CH:21][CH:22]=2)=[C:3]([OH:4])[O:5]1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 737684-(Trifluoromethyl)phenyl isocyanate

Product 1

HCID 22763213HCID 22763213, compound

Reagents, catalysts & solvents 2

HCID 679Dimethyl SulfoxideSolventHCID 962WaterSolvent

Procedure

To a solution of 14.4 g of isopropylidene malonate in 150 ml of dimethyl sulphoxide were added dropwise, at room temperature, 10.1 g of triethylamine and thereafter, at 20° to 30° C., 18.7 g of 4-trifluoromethylphenylisocyanate. The mixture was reacted for 12 to 15 hours at room temperature and the resultant solution was poured into a solution of 15 ml of concentrated hydrochloric acid in 350 ml of water. The precipitate which formed was collected with suction. Recrystallisation from 130 ml of acetone yielded the product of the formula ##STR5## with a melting point of 206°-208° C.

Workup

  1. customat 20° to 30° C.
  2. customThe mixture was reacted for 12 to 15 hours at room temperature
  3. customThe precipitate which formed
  4. customwas collected with suction
  5. customRecrystallisation from 130 ml of acetone
  6. customyielded the product of the formula ##STR5## with a melting point of 206°-208° C.

Sources & evidence

ORD record
ord-d4e87e1e7bc14752a6927b995263320b
Source dataset
uspto-grants-1978_10
Patent number
US04123551

Reaction notes

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