6-Chloro[1,3]dioxolo[4,5-f][1,3]benzothiazole → HCID 178527754, compound
Reaction equation
Cl[C:2]1[S:3][C:4]2[CH:10]=[C:9]3[O:11][CH2:12][O:13][C:8]3=[CH:7][C:5]=2[N:6]=1.NC(N)=[S:16]>C(O)C>[SH:16][C:2]1[S:3][C:4]2[CH:10]=[C:9]3[O:11][CH2:12][O:13][C:8]3=[CH:7][C:5]=2[N:6]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
The product from Step 2 (0.67 g) and thiourea (0.26 g) were mixed in ethanol (20 cm3) and stirred and heated to reflux under an atmosphere of nitrogen for 18 hr. The pale yellow solid which precipitated was filtered from the solution at ambient temperature, washed with ethanol and sucked to dryness to give the required product. 1H NMR (DMSO): δ7.26(1H,s); 6.80(1H,s); 6.02(2H,s); mp 265° C. (dec); M+ =211.
Workup
- temperatureheated
- temperatureto reflux under an atmosphere of nitrogen for 18 hr
- customThe pale yellow solid which precipitated
- filtrationwas filtered from the solution at ambient temperature
- washwashed with ethanol
Sources & evidence
- ORD record
- ord-0d8b9693e20043679f50682ffbbf8374
- Source dataset
- uspto-grants-1995_09
- Patent number
- US05451594
Reaction notes
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