Benzene → HCID 12880034, compound

HRID 2287036Notes

Reaction equation

HRID 2287036 reaction equation
[CH3:1][O:2][CH:3]([O:7][CH3:8])[CH2:4][NH:5][CH3:6].C1C=CC=CC=1.[Cl:15][C:16]1[CH:17]=[C:18]([CH:30]=[C:31]([Cl:33])[CH:32]=1)[O:19][CH:20]([C:22]1[S:26][C:25]([N:27]=[C:28]=[O:29])=[N:24][N:23]=1)[CH3:21]>CCCCCC>[Cl:15][C:16]1[CH:17]=[C:18]([CH:30]=[C:31]([Cl:33])[CH:32]=1)[O:19][CH:20]([C:22]1[S:26][C:25]([NH:27][C:28](=[O:29])[N:5]([CH3:6])[CH2:4][CH:3]([O:7][CH3:8])[O:2][CH3:1])=[N:24][N:23]=1)[CH3:21]

Participants

5

Reactant 3

HCID 241BenzeneHCID 85032,2-DimethoxyethylmethylamineHCID 54545133HCID 54545133, compound

Product 1

HCID 12880034HCID 12880034, compound

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

3.8 grams (0.032 mole) of methylaminoacetaldehyde dimethylacetal was added to a 50 milliliter benzene solution containing 10.0 grams (0.032 mole) of the 5-[1-(3,5-dichlorophenoxy)ethyl]-1,3,4-thiadiazol-2-yl isocyanate dimer (prepared above). The resulting solution was heated to reflux, 50 milliliters of hexane was added, and the solution cooled. The crystals were filtered off, and dried in a vacuum oven at 80° C. to give 7.9 grams of fluffy waxy crystals of 3-[5-[1-(3,5-dichlorophenoxy)ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-1-(2,2-dimethoxyethyl)urea. (Melting point 149°-152° C.).

Workup

  1. additioncontaining
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux
  4. temperaturethe solution cooled
  5. filtrationThe crystals were filtered off
  6. customdried in a vacuum oven at 80° C.

Sources & evidence

ORD record
ord-547fbba6831147648f678c1cdb9a0fda
Source dataset
uspto-grants-1981_05
Patent number
US04268675

Reaction notes

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