Cracking connecting unit for tetrahydrofuran ether derivatives and application of cracking connecting unit
A technology of tetrahydrofuran ether and linking units, which is applied in the fields of chemical synthesis and biochemistry, can solve problems such as insufficient mild cracking conditions, low cracking efficiency, and short read length, and achieve high-efficiency cracking effects
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[0063] Example 1. When n=0, the synthesis of connecting unit T-8
[0064] The schematic diagram of the synthetic route of connecting unit T-8 (5-hydroxymethyl-2-(2-aminoethoxy)-tetrahydrofuran) is as follows figure 1 As shown, the synthesis steps are as follows:
[0065] (1) Synthesis of T-1: D, L or DL-glutamic acid is reacted to obtain T-1 in the presence of sodium nitrite.
[0066] The specific steps are: adding 10 g (68 mmol) of D, L or DL-glutamic acid to a 500 mL single-mouth bottle, adding hydrochloric acid (14 mL of concentrated hydrochloric acid is dissolved in 28 mL of water), and the solid is dissolved. Stir in an ice bath for 30 minutes, and continue to add a solution of sodium nitrite (7 g, 100 mmol, dissolved in 30 mL of water) dropwise in an ice bath. Red-brown smoke is produced during the addition. After the addition is complete, continue to react for 3 hours in an ice bath, and then move to room temperature overnight. The water was evaporated under reduced pressur...
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[0088] Example 2. When n=2, the synthesis of connecting unit T-8'
[0089] Schematic diagram of synthetic route figure 2 As shown, the synthesis steps are as follows:
[0090] (1) The synthesis of T-1 to T-4 is the same as that described in Example 1.
[0091] (2) Synthesis of T-6': T-4 reacts with bromotriethylene glycol to obtain T-6'.
[0092] The specific steps are: take 232 mg of T-4 (1 mmol), add 15 mL of dichloromethane to dissolve, add 426 mg of monobromotriethylene glycol (2 mmol), add 50 mg of Amberlyst A-15, and reflux for 2 hours at 50°C. The reaction was stopped, A-15 was removed by filtration, and washed with saturated sodium bicarbonate and saturated brine. The solvent was evaporated under reduced pressure to obtain 600 mg of light yellow oily liquid. Pack the column with silica gel and separate with petroleum ether: ethyl acetate = 5:1 to obtain 128 mg of pure light green T-6' with a yield of 30%. Cis: 1 H NMR(CDCl 3 , 400M): δ5.17 (1H, d, J=4.8Hz), 4.17~4.08(1H, ...
Example Embodiment
[0098] Example 3. When n=44, the synthesis of connecting unit T-8"
[0099] The schematic diagram of the synthetic route is as image 3 As shown, the synthesis steps are as follows:
[0100] (1) The synthesis of T-1 to T-4 is the same as that described in Example 1.
[0101] (2) Synthesis of T-6": T-4 is reacted with brominated polyethylene glycol 2000 to obtain T-6".
[0102] The specific steps are: take 1 mmol T-4, add 15 mL of dichloromethane to dissolve, add 2 mmol of monobromopolyethylene glycol 2000, add 50 mg of Amberlyst A-15, and reflux for 2 hours at 50°C. The reaction was stopped, A-15 was removed by filtration, and washed with saturated sodium bicarbonate and saturated brine. The solvent was evaporated under reduced pressure to obtain 600 mg of light yellow oily liquid. Pack the column with silica gel and separate with petroleum ether: ethyl acetate = 5:1 to obtain 213 mg of pure light green T-6". 1 H NMR(CDCl 3 , 400M): δ5.19 (1H, d, J=4.8Hz), 4.22~4.19(1H, m), 3.87~3....
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