Thionyl Chloride → HCID 86663089, compound
Reaction equation
[Cl:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH:8]([F:10])[F:9])[C:3]=1[C:11]([OH:13])=O.S(Cl)([Cl:16])=O>>[Cl:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH:8]([F:10])[F:9])[C:3]=1[C:11]([Cl:16])=[O:13]Participants
3
Procedure
3.2 g of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid and 44.3 ml of thionyl chloride are refluxed for 5 hours. After cooling down, the reaction mixture is evaporated under vacuum to yield 3.5 g of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as a yellow oil. 1H NMR (400 MHz, CHCl3-d6) δ ppm: 3.97 (s, 3H); 7.00 (t, J=52.01 Hz, 1H); IR (TQ): 1759 and 1725 cm−1 (C═O).
Workup
- temperatureAfter cooling down
- customthe reaction mixture is evaporated under vacuum
Sources & evidence
- ORD record
- ord-d553d1113d284236ba1afe0a2c7ab97f
- Source dataset
- uspto-grants-2013_12
- Patent number
- US08614242B2
Reaction notes
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