Chlorosulfonic acid → HCID 135838097, compound
Reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[NH2:6][C:7]1[NH:16][C:15](=[O:17])[C:14]2[C:13]3[CH:18]=[CH:19][CH:20]=[CH:21][C:12]=3[CH2:11][CH2:10][C:9]=2[N:8]=1>>[NH2:6][C:7]1[NH:16][C:15](=[O:17])[C:14]2[C:13]3[CH:18]=[CH:19][C:20]([S:2]([Cl:1])(=[O:5])=[O:3])=[CH:21][C:12]=3[CH2:11][CH2:10][C:9]=2[N:8]=1Participants
3
Procedure
Chlorosulfonic acid(25 ml, Aldrich), cooled to 5° C. in ice, was stirred during its addition to 3-amino-1,2,5,6-tetrahydro-1-oxo-benzo [f]quinazoline (5 g, 0.025 mole)contained in a beaker immersed in an ice bath. The solution was removed from the ice bath, stirred for a further 20 min, then poured onto ice (1000 g). The solid product was removed by filtration, washed with water, and dried under high vacuum at room temperature. The sulfonyl chloride was used without further purification.
Workup
- customimmersed in an ice bath
- customThe solution was removed from the ice bath
- additionpoured onto ice (1000 g)
- customThe solid product was removed by filtration
- washwashed with water
- customdried under high vacuum at room temperature
- customThe sulfonyl chloride was used without further purification
Sources & evidence
- ORD record
- ord-6f452deb46d04de0a69893eeb04a3440
- Source dataset
- uspto-grants-2000_07
- Patent number
- US06090941
Reaction notes
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