AMX MAX-CSD 10 Bedienungsanleitung PDF herunterladen (Seite 3)

A mixture of dimethyl 5-hydroxyisophthalate (2.10 g, 10.0 mmol), trans-1,4-dibromobut-2-ene

(1.05 g, 4.90 mmol), K

(2.21 g, 16.0 mmol) and dibenzo-18-crown-6 (0.10 g, 0.277 mmol)

were stirred in dry THF (40 ml) under N

at 65 ºC for 24 hours. After this time, a solution of 1 %

aqueous Na

(20 ml) was added at 0 ºC. The resulting solid was collected, washed with water

and ether and dried under vacuum to give 2.17 g (94 %) of the butenetetraester Me

L2 as a white

solid.

IR (ATR): ν 1719 cm

-1

(carbonyl)

H NMR (CDCl

): δ 3.92 (s, 12H), 4.68 (dd, 4H), 6.10 (dt, 2H), 7.75 (d, 4H), 8.26 (t, 2H)

C NMR (CDCl

): δ 52.48, 67.95, 120.00, 123.24, 128.00, 131.79 (no 4º carbon signals

observed)

MS (ESI+): m/z calcd for C

472, found 472

2.4 Butene Tetraacid (H

L2)

A mixture of butene tetraester Me

L2 (1.00 g, 2.12 mmol), KOH (0.475 g, 8.46 mmol), methanol

(15 ml) and distilled water (15 ml) were stirred under N

at 60 ºC for 48 hours. After this time,

the reaction mixture was filtered to remove any unreacted starting materials. HCl (6 M, 25 ml)

was then added dropwise at 0 ºC. The precipitate was collected, washed with water and dried

under vacuum to give 0.556 g (63 %) of butenetetraacid H

L2 as a white solid.

IR (ATR): ν 1686 cm

-1

(carbonyl)

H NMR (d

-DMSO): δ 4.73 (s, 4H), 6.11 (s, 2H), 7.66 (s, 4H), 8.06 (s, 2H), 13.30 (br, 4H)

C NMR (d

-DMSO): δ 67.67, 119.28, 122.38, 132.58, 158.27, 166.32

MS (ESI-): m/z calcd for C

416, found 415 [M – H]

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