Bromine → HCID 54019409, compound

HRID 2351249Notes

Reaction equation

HRID 2351249 reaction equation
[K].[CH2:2]([O:4][C:5]([C:7]1[CH:8]=[N:9][N:10]([CH3:29])[C:11]=1[S:12]([NH:15][C:16]([NH:18][C:19]1[N:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[N:20]=1)=[S:17])(=[O:14])=[O:13])=[O:6])[CH3:3].BrBr>N1C=CC=CC=1>[CH3:26][O:25][C:23]1[CH:22]=[C:21]([O:27][CH3:28])[N:20]2[S:17][C:16](=[N:15][S:12]([C:11]3[N:10]([CH3:29])[N:9]=[CH:8][C:7]=3[C:5]([O:4][CH2:2][CH3:3])=[O:6])(=[O:13])=[O:14])[N:18]=[C:19]2[N:24]=1

Participants

5

Reactant 3

HCID 24408BromineHCID 5462222PotassiumHCID 14152126HCID 14152126, compound

Product 1

HCID 54019409HCID 54019409, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

0 g of potassium salt of N-(4-ethoxycarbonyl-1-methyl-5-pyrazolesulfonyl)-N'-(4,6-dimethoxy-2-pyrimidinyl)thiourea (acetonitrile-solvate product) is dissolved in 20 ml of pyridine, and to the solution is added dropwise 0.37 g of bromine while cooling at -6° C. to -8° C. The reaction mixture is stirred at the same temperature for 2 hours, and poured into 100 ml of ice water. The resulting crystals are filtered, washed with water, and recrystallized from acetonitrile to give 0.5 g of the title compound as colorless crystals.

Workup

  1. temperaturewhile cooling at -6° C. to -8° C
  2. filtrationThe resulting crystals are filtered
  3. washwashed with water
  4. customrecrystallized from acetonitrile

Sources & evidence

ORD record
ord-673e648f50d64713b27b635a884c6247
Source dataset
uspto-grants-1989_10
Patent number
US04872901

Reaction notes

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