Triethylamine → HCID 12684545, compound

HRID 2420075Notes

Reaction equation

HRID 2420075 reaction equation
Cl.[CH3:2][NH:3][OH:4].C(N(CC)CC)C.[Cl:12][C:13]1[CH:14]=[C:15]([N:20]=[C:21]=[O:22])[CH:16]=[C:17]([Cl:19])[CH:18]=1>C(Cl)(Cl)Cl>[CH3:2][N:3]([OH:4])[C:21]([NH:20][C:15]1[CH:16]=[C:17]([Cl:19])[CH:18]=[C:13]([Cl:12])[CH:14]=1)=[O:22]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 77906N-methylhydroxylamine hydrochlorideHCID 944603,5-Dichlorophenyl isocyanate

Product 1

HCID 12684545HCID 12684545, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent2×

Conditions

Temperature
20 °C

Procedure

A mixture of 10 g of N-methyl-hydroxylamine hydrochloride in 100 ml of chloroform was stirred while 18 ml of triethylamine were added at 0° C. Then, 20 g of 3,5-dichlorophenyl isocyanate in 30 ml of chloroform were added to the mixture at 10° to 15° C and the mixture was stirred for 5 hours at 20° C and was then distilled to dryness under reduced pressure. The residue was taken up in water and dried to obtain 22 g of N-methyl-N-hydroxy-N'-(3,5-dichlorophenyl)-urea melting at 131°-132° C.

Workup

  1. additionwere added at 0° C
  2. distillationwas then distilled to dryness under reduced pressure
  3. customdried

Sources & evidence

ORD record
ord-0ae5cc9b564a47e7bdc7a0050e5653c9
Source dataset
uspto-grants-1978_08
Patent number
US04108993

Reaction notes

Loading…