반응 #63706

반응 방정식

N3CF2CF2C(ONa)(OCH2CF3)CF3

dimethyl sulfate

→

6-azido-4-methoxy-4-trifluoromethyl-1,1,1,5,5,6,6-hepta fluoro-3-oxahexane

수율 72.0%

반응 조건

후처리

1. 1
   온도heated to 40° (0.5 mm, 0.1 kPa)
2. 2
   기타to remove volatiles

실험 절차

To demonstrate that the product was N3CF2CF2C(ONa)(OCH2CF3)CF3, the reaction mixture was stirred overnight with 56.7 g (0.45 mol) of dimethyl sulfate, then heated to 40° (0.5 mm, 0.1 kPa) to remove volatiles. Fractionation of the volatiles gave 101.4 g (72%) of 6-azido-4-methoxy-4-trifluoromethyl-1,1,1,5,5,6,6-hepta fluoro-3-oxahexane, bp 60°-61° (15 mm, 2.0 kPa). IR (CCl4): 3010, 2970, and 2660 (sat'd CH), 2150 (N3), 1300-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 4.10 (q, JFF 7.8 Hz, 2H, CH2CF3) and 3.67 ppm (s, 3H, OCH3); 19F-73.8 (t of t, JFF 9.3, 7.9 Hz, 3F, CF3), -75.3 (t, JHF 7.8 Hz, 3F, CF3CH2), -89.3 (q or t, JFF 7.9, 3.4 Hz, 2F, CF2N3), and 117.7 ppm (q of t, JFF 9.3, 3.4 Hz, CF2).

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