반응 #2155847

반응 방정식

HATU

5-oxazol-4-yl-thiophene-3-carboxylic acid

4,4-Difluoro-azepane trifluoroacetate

DIPEA

→

title compound

수율 30.9%

(4,4-Difluoro-azepan-1-yl)-(5-oxazol-4-yl-thiophen-3-yl)-methanone

수율 30.9%

용매

DCM

THF

반응 조건

후처리

1. 1
   세척then washed with aqueous sodium carbonate solution
2. 2
   건조The organics were dried over sodium sulfate
3. 3
   여과filtered
4. 4
   기타evaporated
5. 5
   기타The crude material was purified by HPLC
6. 6
   세척eluting with 5%-98% methanol in water (0.1% formic acid)
7. 7
   workup.ADDITIONThe fractions containing the desired product
8. 8
   기타were freeze-dried

실험 절차

4,4-Difluoro-azepane trifluoroacetate (Synthesis 47, 0.113 g, 0.45 mmol) was dissolved in THF (1 mL) and added to 5-oxazol-4-yl-thiophene-3-carboxylic acid (0.059 g, 0.30 mmol). DIPEA (0.154 mL, 0.90 mmol) was added followed by HATU (0.125 g, 0.33 mmol) and the reaction mixture was then stirred at room temperature overnight. The mixture was diluted with DCM then washed with aqueous sodium carbonate solution. The organics were dried over sodium sulfate, filtered and evaporated. The crude material was purified by HPLC, eluting with 5%-98% methanol in water (0.1% formic acid). The fractions containing the desired product were freeze-dried to give the title compound (0.029 g). LCMS m/z 313.15 [M+H]+ R.T.=8.31 min (Analytical Method 10).

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