Sulfur Dioxide → HCID 22476014, compound
Reaction equation
[NH:1]1[CH2:6][CH2:5][CH2:4][N:3]=[C:2]1[NH:7][C:8]([CH2:10][CH2:11][C:12]1[CH:20]=[CH:19][C:15]([C:16](O)=[O:17])=[CH:14][CH:13]=1)=[O:9].S(Cl)([Cl:23])=O.S(=O)=O>C1(C)C=CC=CC=1>[ClH:23].[NH:1]1[CH2:6][CH2:5][CH2:4][N:3]=[C:2]1[NH:7][C:8]([CH2:10][CH2:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([Cl:23])=[O:17])=[CH:14][CH:13]=1)=[O:9]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 70 °C
Procedure
110.2 g (0.4 mol) of 4-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)ethyl)benzoic acid were suspended in 1.5 l of toluene, then 35 ml of thionyl chloride were added and the mixture was heated to 70° C. for 2 h. Then further 16 ml of thionyl chloride were added and heating was continued until the evolution of sulfur dioxide had ceased. The almost clear solution was evaporated to dryness to give 139.5 g of the crude title compound as a yellow powder. This product was directly used in the subsequent reaction.
Workup
- temperatureheating
- customThe almost clear solution was evaporated to dryness
Sources & evidence
- ORD record
- ord-15dd10c798674f929ead3b116301de95
- Source dataset
- uspto-grants-2005_05
- Patent number
- US06900318B1
Reaction notes
Loading…