Potassium Carbonate → HCID 67236548, 화합물

Methyl 2-bromobenzo[d]thiazole-6-carboxylate (0.52 g, 1.90 mmol), Boc-piperazine (0.44 g. 2.38 mmol) and potassium carbonate (0.53 g, 3.80 mmol) were suspended in acetonitrile (21 ml) and refluxed overnight. The resulting mixture was then cooled to room temperature, concentrated in vacuo to approximately 2 ml, diluted with water and extracted with ethyl acetate. The organic layer was dried (MgSO4) and concentrated in vacuo to yield a residue which was treated with trifluoroacetic acid/dichloromethane (6 ml, 1:1) for 1.5 hrs. The resulting mixture was concentrated in vacuo, the resulting residue was dissolved in dichloromethane and washed with saturated sodium bicarbonate to yield methyl 2-(piperazin-1-yl)benzo[d]thiazole-6-carboxylate.

1. temperaturerefluxed overnight
2. concentrationconcentrated in vacuo to approximately 2 ml
3. additiondiluted with water
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto yield a residue which
8. concentrationThe resulting mixture was concentrated in vacuo
9. dissolutionthe resulting residue was dissolved in dichloromethane
10. washwashed with saturated sodium bicarbonate

ORD 기록

ord-67529be9aa914bdfa4b8f415c0ecf444

출처 데이터셋

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08481547B2