* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
A mixture of the above foam (120 mg, 0.9 mmol) and POCl3 (5 mL) was heated to 120° C. for 6 h and then concentrated in vacuo. The residue was diluted with EtOAc and washed with saturated aqueous NaHCO3. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo to give the desired compound as tan solid (50 mg, 36percent yield, which was used directly for the next step). MS: (ES) m/z 155.0 (M+H+).
Reference：
[1] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1980, p. 506 - 511
[2] Patent: US2014/154179, 2014, A1, . Location in patent: Paragraph 0412; 0417
2
[ 399-66-6 ]
[ 74803-32-0 ]
Reference：
[1] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1980, p. 506 - 511
[2] Patent: US2014/154179, 2014, A1,
A mixture of the above foam (120 mg, 0.9 mmol) and POCl3 (5 mL) was heated to 120 C. for 6 h and then concentrated in vacuo. The residue was diluted with EtOAc and washed with saturated aqueous NaHCO3. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo to give the desired compound as tan solid (50 mg, 36% yield, which was used directly for the next step). MS: (ES) m/z 155.0 (M+H+).
With N,N-diethyl-N-isopropylamine; at 120.0℃; for 2.0h;
A mixture of the above <strong>[74803-32-0]8-chloro-[1,2,4]triazolo[1,5-a]pyrazine</strong> (50 mg, 0.32 mmol) and (S)-tert-butyl pyrrolidin-3-yl carbamate (100 mg, 0.53 mmol) in diethylisopropylamine (2 mL) was heated to 120 C. for 2 h. After coolingto room temperature, the mixture was diluted with 10%MeOH in EtOAc and washed with saturated aqueous solutionsof KH2PO4 and NaHCO3, followed by brine. The organic layer was concentrated in vacuo and the residue purified by flash chromatography (Si02, 2 to 5% MeOH in CH2C12 as eluent) to give the desired compound as a foam (80mg, 82% yield, which was used directly for the next step). MS: (ES) m/z 305.2 (M+H+).
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