Triethylamine → HCID 12225680, compound

HRID 2420077Notes

Reaction equation

C(N(CC)CC)C.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]=[C:16]=[O:17])=[CH:11][C:10]=1[C:18]([F:21])([F:20])[F:19].Cl.[CH3:23][NH:24][OH:25]>C(Cl)(Cl)Cl>[CH3:23][N:24]([OH:25])[C:16]([NH:15][C:12]1[CH:13]=[CH:14][C:9]([Cl:8])=[C:10]([C:18]([F:19])([F:20])[F:21])[CH:11]=1)=[O:17]

Participants

Conditions

Temperature: 20 °C

Procedure

33 ml of triethylamine and then 44.3 g of 4-chloro-3-trifluoromethylphenyl isocyanate in 200 ml of chloroform were added to a mixture of 21 g of N-methyl hydroxylamine hydrochloride and 200 ml of chloroform at 0° C and the mixture was stirred at 20° C for 16 hours. The mixture was washed with water and was reduced to a volume of 100 ml under reduced pressure. The mixture was iced and vacuum filtered. The crystals were washed with water and dried to obtain 37 g of N-methyl-N-hydroxy-N'-(4'-chloro-3'-trifluoromethylphenyl)-urea melting at 114°-115° C.

Workup

washThe mixture was washed with water
filtrationvacuum filtered
washThe crystals were washed with water
customdried

Sources & evidence

ORD record: ord-af6f491cb0df42d898fc44f404653d51
Source dataset: uspto-grants-1978_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04108993

Reaction notes

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