3,5-Dimethylpyrazole → HCID 70540275, compound

HRID 1105885Notes

Reaction equation

[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](=[O:15])[CH:13](Br)[C:12]([NH:17][C:18](=[O:39])[CH2:19][CH2:20][CH2:21][O:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([CH2:32][CH3:33])([CH3:31])[CH3:30])=[CH:25][C:24]=2[C:34]([CH2:37][CH3:38])([CH3:36])[CH3:35])=[N:11]1.[CH3:40][C:41]1[CH:45]=[C:44]([CH3:46])[NH:43][N:42]=1>C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](=[O:15])[CH:13]([C:45]2[C:41]([CH3:40])=[N:42][NH:43][C:44]=2[CH3:46])[C:12]([NH:17][C:18](=[O:39])[CH2:19][CH2:20][CH2:21][O:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([CH2:32][CH3:33])([CH3:31])[CH3:30])=[CH:25][C:24]=2[C:34]([CH2:37][CH3:38])([CH3:36])[CH3:35])=[N:11]1

Participants

Conditions

Temperature: 100 °C

Procedure

66 g of 1-(2,4,6-trichlorophenyl)-3-[4-(2,4-di-tert-amylphenoxy)butyramido]-4-bromo-5-oxo-2-pyrazoline and 27 g of 3,5-dimethylpyrazole were mixed well with each other in a mortar, then stirred for 2 hours under heating at 100° C. To the reaction mixture was added 1 liter of ethyl acetate followed by washing several times with water. The ethyl acetate layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from ethyl acetate, 35 g of Coupler (1) was obtained. The melting point of the coupler was 207° to 209° C.

Workup

washby washing several times with water
dry with materialThe ethyl acetate layer was dried with anhydrous sodium sulfate
concentrationconcentrated
customUpon crystallization of the residue from ethyl acetate, 35 g of Coupler (1)
customwas obtained
customwas 207° to 209° C.

Sources & evidence

ORD record: ord-cadd0c71fdc949d7b55f5f95ad89c2c3
Source dataset: uspto-grants-1982_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04310619

Reaction notes

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