A general and expedient method for the solid-phase synthesis of 1,4-benzodiazepine derivatives, Journal of the American Chemical Society, vol.114, issue.27, p.10997, 1992. ,
DOI : 10.1021/ja00053a067
Recoverable Catalysts and Reagents Using Recyclable Polystyrene-Based Supports, Chemical Reviews, vol.102, issue.10, p.3275, 2002. ,
DOI : 10.1021/cr0103571
Soluble polymer supports for liquid-phase synthesis, Adv. Polym. Sci, vol.121, p.31, 1995. ,
DOI : 10.1007/BFb0018578
Synthesis and conformation of a polyoxyethylene-bound undecapeptide of the alamethicin helix and (2-methylalanyl-L-alanine)1-7, Biopolymers, vol.16, issue.2, p.425, 1979. ,
DOI : 10.1002/bip.1979.360180217
40 (s, 2 H, H-6), 6.04 (s, 2 H, H-8a), 6.15 (s, 2 H, pp.50-53 ,
52-3.63 (m, 1 H, H-7), 4.88 (d, J 6-7 = 7.0 Hz, 0, p.338 ,
41 (ddd, J 4eq-2eq = 1.5 Hz, 1 H, H-4eq), 3.90 (d, J 1'a-1'b = 13.5 Hz, 1 H, H-1'a), 3.92 (s, 3 H, CH 3 ), 4.04 (d, 1 H, H-1'b), pp.31-35 ,
50 (d, J 2"-3" = 8.5 Hz, p.9 ,
94 (s, 3 H, CH 3 ), 4.48 (d, J 2ax-2eq = 10.5 Hz, 1 H, H-2ax), 4.60 (d, J 6ax-5 = 10, Hz, 1 H, H-6ax), 4.69 (dd, p.9 ,
30 (dd, J 10a-10b = 14.0 Hz, J 10a-11 = 6.5 Hz, 2 H, H-10a), 3.38 (dd, pp.4-45, 2002. ,
19 (dd, J 4ax-4eq = 13.5 Hz, J 4ax- 5eq = 3.5 Hz, 1.5 H, H-4ax major), 3.35-3.89 (m, 256 H, PEG backbone, H-4eq minor, H-4ax minor, H-4eq major, pp.4-48 ,
25 (dd, J 3'e-2' = 9.5 Hz, J 3'e-3'z = 1.0 Hz, 2 H, H-3'e), 5.35 (dd, J 3'z-2' = 15 Hz, pp.77-82 ,
58 (dm, 1 H, H-4eq), 3.61 (dd, J 1'a-1'b = 13.5 Hz, J 1'a-2' = 6.5 Hz, 1 H, H-1'a), 3.65 (dd, J 1'b-2' = 6.5 Hz, pp.3-94 ,
32 (dd, J 4ax-4eq = 13 ,
1.5 Hz, 1 H, H-4eq), 3.53 (dd, J 1'b-2' = 6.5 Hz, 1 H, H-1'b), 3.95 (s, 3 H, CH 3, pp.50-54 ,
Compound 37c To 1 mL solution of MeONa in MeOH (0.1 M), compound 37b (550 mg, 0.21 mmol), was added. The reaction mixture was stirred at room temperature for 3 hours, mL of CH 3 COOH in MeOH (0.1 M) was added and the mixture was stirred at room temperature for 10 min ,
:3) to give 37c (45 mg, 37 %) as white foam (m, °C), and 37d (24 mg, 20 %) as colorless oil, pp.138-140 ,
64 (ddd, J 4eq-2eq(W) = 2.0 Hz, 1 H, H-4eq), 3.65 (dd, J 1'a-1'b = 17.0 Hz, 1 H, H-1'a), 3.70 (dd, 1 H, H-1'b), 3.94 (s, 3 H, CH 3, pp.4-74 ,
27 (dd, J 4ax-4eq = 13.5 Hz, J 4ax-5eq = 3.5 Hz, 1.5 H, H-4ax major), 3.37-3.44 (m, 2 H, H-4ax minor, H-4eq minor), 3.49 (dm, 1, pp.3-53 ,
1.5 Hz 140 (d, J 3'-4' = 8.0 Hz, 0.5 H, H-3' minor), 7.50 (d, J 2, pp.4-86, 2002. ,
Compound 38c To 2 mL solution of MeONa in MeOH (0.1 M), compound 38b (1.36 g, 0.5 mmol), was added. The reaction mixture was stirred at room temperature for 3 hours, mL of CH 3 COOH in MeOH (0.1 M) was added and the mixture was stirred at room temperature for 10 min ,
48 (dm, 1 H, H-4eq), 3.89 (s, 3 H, CH 3 ,
4.24 (d, 1 H, H-1'b), 4.41 (d, J 2ax-2eq = 10, Hz, vol.1, pp.4-72 ,
34-3.44 (m, 2 H, H-4ax, H-4eq), 3.91 (s, 3 H, CH 3 ,