Hydrochloric Acid → HCID 11173741, compound

HRID 1267581Notes

Reaction equation

HRID 1267581 reaction equation
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[CH:10]([C:14]([NH2:16])=[O:15])[C:11]([NH2:13])=[O:12].Br.Br.[O:19]1[CH2:25][CH2:24]NN[CH2:21][CH2:20]1.C(N(CC)CC)C.Cl>C1(C)C(C)=CC=CC=1>[CH3:9][C:4]1[CH:5]=[C:6]([CH3:8])[CH:7]=[C:2]([CH3:1])[C:3]=1[CH:10]1[C:11](=[O:12])[N:13]2[CH2:21][CH2:20][O:19][CH2:25][CH2:24][N:16]2[C:14]1=[O:15]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 11481413HCID 11481413, compoundHCID 18546776HCID 18546776, compound

Product 1

HCID 11173741HCID 11173741, compound

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Conditions

Temperature
22 °C

Procedure

A solution of 1.5 g (0.0068 mol) of 2,4,6-trimethylphenylmalonic acid diamide, 2.16 g (0.0082 mol) of [1,4,5]oxadiazepane dihydrobromide and 2.93 g (0.029 mol) of triethylamine. in 50 ml of xylene is heated for two hours at reflux temperature in a nitrogen atmosphere. The suspension formed is cooled to 22° C., stirred with 1N hydrochloric acid and filtered. The crystalline residue is washed with water and then with diethyl ether and dried in vacuo at 60° C. The desired title compound has a melting point of 248-250° C.

Workup

  1. temperatureat reflux temperature in a nitrogen atmosphere
  2. customThe suspension formed
  3. filtrationfiltered
  4. washThe crystalline residue is washed with water
  5. dry with materialwith diethyl ether and dried in vacuo at 60° C

Sources & evidence

ORD record
ord-5ecf1bc6c6004da1b6716f3e7ea6c709
Source dataset
uspto-grants-2003_04
Patent number
US06552187B1

Reaction notes

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