Ethanethiol → HCID 13317020, compound
Reaction equation
CC(C)([O-])C.[K+].[CH2:7]([SH:9])[CH3:8].Cl[C:11]1[N:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][N:12]=1>C(COC)OC>[CH2:7]([S:9][C:11]1[N:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][N:12]=1)[CH3:8]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Potassium tert-butoxide (8.9 mmol) was added to an ice-cooled solution of ethanethiol (8.9 mmol) in dimethoxyethane (40 ml) and the mixture stirred at room temperature for 10 min before 2-chloro-5-trifluoromethylpyrimidine (8.9 mmol) in dimethoxyethane (10 ml) was added. The resultant mixture was stirred at room temperature for 2 h and at 80° C. for 30 mins. The solvent was then removed at reduced pressure and the residue distilled; yield 1.40 g (76%), b.p. 110°-112° C./40 mmHg. 1H NMR (CDCl3): δ 1.41 and 3.21 (Et), 8.65 (H-4 and H-6).
Workup
- additionwas added
- customThe solvent was then removed at reduced pressure
- distillationthe residue distilled
Sources & evidence
- ORD record
- ord-04c6a0564c964b17b1883c0f8de22133
- Source dataset
- uspto-grants-1986_06
- Patent number
- US04596870
Reaction notes
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