Hexane → HCID 13083045, compound

HRID 325254Notes

Reaction equation

HRID 325254 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[N:5]=[C:4]([CH3:10])[N:3]=1.[Cl:11][C:12]([Cl:22])([Cl:21])[CH2:13][O:14][S:15]([N:18]=[C:19]=[O:20])(=[O:17])=[O:16].CCCCCC>ClCCl>[CH3:9][O:8][C:6]1[N:5]=[C:4]([CH3:10])[N:3]=[C:2]([NH:1][C:19]([NH:18][S:15]([O:14][CH2:13][C:12]([Cl:22])([Cl:21])[Cl:11])(=[O:16])=[O:17])=[O:20])[N:7]=1

Participants

5

Reactant 3

HCID 8058HexaneHCID 154662-Amino-4-methoxy-6-methyl-1,3,5-triazineHCID 11322793HCID 11322793, compound

Product 1

HCID 13083045HCID 13083045, compoundYield 89.5%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

14.0 g (0.1 mole) of 2-amino-4-methoxy-6-methyl-1,3,5-triazine were suspended in 250 ml of dichloromethane, and a solution of 25.5 g (0.1 mole) of 2,2,2-trichloro-eth-1-oxysulfonyl isocyanate in 100 ml of dichloromethane was added dropwise at 0° to 5° C. The reaction mixture was further stirred for 18 hours at room temperature and cooled to 0° C., and n-hexane was added. The precipitated reaction product was filtered off under suction and recrystallized from absolute ethanol. 35.3 g (89.4% of theory) of N-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-N'-(2,2,2-trichloro-eth-1-oxy-sulfonyl)-urea of melting point 128° C. were obtained.

Workup

  1. temperaturecooled to 0° C.
  2. customThe precipitated reaction product
  3. filtrationwas filtered off under suction
  4. customrecrystallized from absolute ethanol

Sources & evidence

ORD record
ord-a91458f73cbc4896a6936a8c0c7c8ad7
Source dataset
uspto-grants-1984_04
Patent number
US04440565

Reaction notes

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