Hydrochloric Acid → HCID 14053356, compound

HRID 652062Notes

Reaction equation

HRID 652062 reaction equation
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=[O:7])[N:5]([CH2:11][CH3:12])[C:3]1=[S:4].C(N(CC)CC)C.[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([N:27]=[C:28]=[O:29])=[C:23]([O:30][C:31]2[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=2)[CH:22]=1.Cl>C1(C)C(C)=CC=CC=1>[CH3:1][N:2]1[C:9](=[O:10])[CH:8]([C:28](=[O:29])[NH:27][C:24]2[CH:25]=[CH:26][C:21]([Cl:20])=[CH:22][C:23]=2[O:30][C:31]2[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=2)[C:6](=[O:7])[N:5]([CH2:11][CH3:12])[C:3]1=[S:4]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14053354HCID 14053354, compoundHCID 14053355HCID 14053355, compound

Product 1

HCID 14053356HCID 14053356, compound

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent2×

Conditions

Temperature
40 °C

Procedure

3.4 g (20 mmol) of 1-methyl-3-ethyl-2-thiobarbituric acid are suspended in 80 ml of xylene. 1 g (8 mmol) of triethylamine is added, the mixture is heated to 40° C. and a solution of 5.6 g (20 mmol) of 4-chloro-2-(4-chlorophenoxy)phenylisocyanate in 30 ml of xylene is added dropwise with stirring at 40° C. The mixture is subsequently stirred for 2 hours at 40° C. and then cooled. 50 ml of 2N HCl are added, the crystalline precipitate is isolated by filtration, washed with water and dried at 80° C., affording a product with a melting point of 250°-251° C.

Workup

  1. stirringThe mixture is subsequently stirred for 2 hours at 40° C.
  2. temperaturecooled
  3. customthe crystalline precipitate is isolated by filtration
  4. washwashed with water
  5. customdried at 80° C.
  6. customaffording a product with a melting point of 250°-251° C.

Sources & evidence

ORD record
ord-1bb3513d48b14d469f15d8a9ca53cb4e
Source dataset
uspto-grants-1987_06
Patent number
US04670441

Reaction notes

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