Isopropanol → HCID 21249242, compound
Reaction equation
Cl.[CH3:2][C:3]1[C:7]2[CH:8]=[C:9]([NH2:13])[CH:10]=[C:11]([F:12])[C:6]=2[S:5][CH:4]=1.[N:14]([O-])=O.[Na+].O.O.[Cl:20][Sn]Cl.C(O)(C)C>O.Cl>[ClH:20].[CH3:2][C:3]1[C:7]2[CH:8]=[C:9]([NH:13][NH2:14])[CH:10]=[C:11]([F:12])[C:6]=2[S:5][CH:4]=1Participants
7
Procedure
0.1 mole of 3-methyl-7-fluoro-5-aminobenzothiophene hydrochloride is suspended in 100 ml of water and 100 ml of concentrated hydrochloric acid, and a solution of 0.11 mole of sodium nitrite in 50 ml of water is added dropwise at between -5° C. and 0° C. The diazonium salt solution is added dropwise to a mixture, cooled to 0° C., of 0.21 mole of SnCl2.2H2O and 200 ml of concentrated hydrochloric acid. After the mixture has been warmed to room temperature, 60 ml of isopropanol are added and the crystal mass is filtered off with suction and recrystallised from isopropanol.
Workup
- filtrationthe crystal mass is filtered off with suction
- customrecrystallised from isopropanol
Sources & evidence
- ORD record
- ord-1fe6357c6b2447b68dcb271fd301ab41
- Source dataset
- uspto-grants-1989_03
- Patent number
- US04816461
Reaction notes
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