HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → N-Methyl-2-(6-methylaminopyridin-3-yl)benzothiazol-6-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | 2-Amino-6-benzothiazolol | HCID 33462 | — |
| Product | N-Methyl-2-(6-methylaminopyridin-3-yl)benzothiazol-6-amine | HCID 24804556 | — |
Reaction Steps
A solution of 2-amino-6-hydroxybenzothiazole (5.00 g, 30.1 mmol), TBDMSCl (5.40 g, 1.2 equiv) and imidazole (2.46 g, 1.2 equiv) in DMF (160 ml) was stirred at ambient temperature for 16 h. The reaction mixture was then partitioned between water and ethyl acetate. The aqueous phase was extracted twice with ethyl acetate and the combined organics dried (MgSO4) and concentrated in vacuo. The crude product thus obtained was purified by silica gel chromatography by gradient elution (Q-heptane:ethyl acetate) to yield 3.0 g of the title compound as a yellowish solid. 1H NMR δ 7.23 (br s, 2H) 7.18 (d, 1H) 7.16 (d, 1H) 6.70 (dd, 1H) 0.95 (s, 9H) 0.16 (s, 6H); MS m/z (M+H) 281.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163928B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-1f56b7fd2ad74233bff0a4622d4dced7 |
| Source note | uspto-grants-2012_04 |