AMX MAX-CSD 10 Manual de usuario descargar pdf (Pagina 2)

A mixture of dimethyl 5-hydroxyisophthalate (2.43 g, 11.6 mmol), 1,4-dibromobutane (1.08 g,

5.00 mmol) and K

(2.50 g, 18.1 mmol) were stirred in DMF (40 ml) at room temperature for

48 hours. After this time, the reaction mixture was poured into water (~400 ml) and stirred for a

further 15 minutes. The resulting white precipitate was collected and washed three times with

water. The precipitate was dissolved in CH

(~150 ml) and then washed with a solution of 5 %

aqueous NaOH solution (2 x 100 ml portions). The CH

solution was then dried over MgSO

filtered and reduced to give 1.79 g (75 %) of the butanetetraester Me

L1 as a white solid.

IR (ATR): ν 1723 cm

-1

(carbonyl)

H NMR (CDCl

): δ 2.02 (m, 4H), 3.93 (s, 12H), 4.12 (m, 4H), 7.71 (d, 4H), 8.26 (t, 2H)

C NMR (CDCl

): δ 25.78, 52.44, 67.94, 119.79, 122.95, 131.73 (no 4º carbon signals

observed)

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

474, found 474

2.2 Butane Tetraacid (H

L1)

A mixture of butane tetraester Me

L1 (1.50 g, 3.16 mmol), KOH (0.710 g, 12.7 mmol), methanol

(25 ml) and distilled water (25 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 1.04 g (79 %) of butanetetraacid H

L1 as a white solid.

IR (ATR): ν 1671 cm

-1

(carbonyl)

H NMR (d

-DMSO): δ 1.91 (s, 4H), 4.15 (s, 4H), 7.63 (d, 4H), 8.06 (t, 2H), 13.27 (br, 4H)

C NMR (d

-DMSO): δ 25.62, 68.17, 119.53, 122.62, 132.98, 159.22, 166.83

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

418, found 417 [M – H]

Elemental Analysis: calcd for C

C 57.42 % H 4.54 % found C 56.75 % H 4.18 %

2.3 Butene Tetraester (Me

L2)

1 2 3 4 5 6 7 ... 10 11

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