반응 #67202

반응 방정식

[(2S)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methylamine

1,1,1-trifluoro-3-iodopropane

→

N-{[(2S)-7-(METHYLSULFONYL)-2,3-DIHYDRO-1,4-BENZODIOXIN-2-YL]METHYL}-N-(3,3,3-TRIFLUOROPROPYL)AMINE

용매

ACN

반응 조건

후처리

1. 1
   기타The product was evaporated to dryness
2. 2
   기타was purified by preparative HPLC (MeOH/NH3 buffer)
3. 3
   기타was crystallized from MeOH/Et2O
4. 4
   기타[α]=−52° (MeOH)

실험 절차

A mixture of [(2S)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methylamine (0.31 g, 1.27 mmol), 1,1,1-trifluoro-3-iodopropane (0.16 ml, 1.4 mmol) K2CO3 (0.35 g, 2.5 mmol) and ACN (4 ml) was heated under microwave radiation at 120° C. for 40 min. The product was evaporated to dryness and was purified by preparative HPLC (MeOH/NH3 buffer). Yield: 0.19 g, 44%. The amine was converted to the hydrochloric acid salt and was crystallized from MeOH/Et2O. M.p. 204° C. MS m/z (rel. intensity, 70 eV) 339 (M+, 3), 127 (5), 126 (bp), 79 (4), 51 (4). [α]=−52° (MeOH).

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