* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
1 Synthesis of C-1
Under a stream of nitrogen AzC-1 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210 . Then filter the solid salt after the completion of the reaction, the reaction was purified by column chromatography to give the title compound 1-C (2.9 g, 65% yield).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
6 Synthesis of C-6
Under a stream of nitrogen AzC-2 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210 . Then filter the solid salt after the completion of the reaction was purified by column chromatography to give the desired compound of our 6-C (2.9 g, yield 66%).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
11 Synthesis of C-11
Under a stream of nitrogen AzC-3 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . Then filter the solid salt after the completion of the reaction, the reaction was purified by column chromatography to give the title compound 11-C (3.0 g, yield 67%).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
16 Synthesis of C-16
Under a stream of nitrogen AzC-4 (2.9 g, 6.7 mmol) ,4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210 . After the solid salt after the reaction was terminated to obtain a filter column 16-C (2.9 g, yield 65%) and chromatographed to give the desired compound.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
21 Synthesis of C-21
Under a stream of nitrogen AzC-5 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . Then filter the solid salt after the completion of the reaction, the reaction was purified by column chromatography to give the title compound 21-C (2.7 g, 61% yield).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
26 Synthesis of C-26
Under a stream of nitrogen AzC-6 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 26-C (3.1 g, yield 69%)
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
31 Synthesis of C-31
Under a stream of nitrogen AzC-7 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 31-C (3.1 g, yield 70%).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
36 Synthesis of C-36
Under a stream of nitrogen AzC-8 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 36-C (2.9 g, yield 66%).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
41 Synthesis of C-41
Under a stream of nitrogen AzC-9 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 41-C (2.7 g, yield 60%)
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
46 Synthesis of C-46
Under a nitrogen flow AzC-10 (2.9 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt C-46 column and purified by chromatography to give the objective compound (3.2 g, yield 71%) was obtained
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
51 Synthesis of C-51
Under a stream of nitrogen AzC-11 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was completed, the C-51 to give the desired compound as a solid after salt filter column chromatography (2.7 g, yield: 61%) to give
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
56 Synthesis of C-56
Under a stream of nitrogen AzC-12 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . C-56 to give the desired compound by column chromatography After the reaction was terminated after filter the solid salt (3.1 g, yield 69%) was obtained
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
61 Synthesis of C-61
Under a nitrogen flow AzC-13 (2.9 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210 . After the reaction was terminated after filter the solid salt to obtain a column-61 C (3.2 g, yield 72%) of the desired compound purified by chromatography.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
66 Synthesis of C-66
Under a stream of nitrogen AzC-14 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated to obtain a solid salt filter and then column C-66 (2.8 g, yield 63%) of the desired compound purified by chromatography.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
71 Synthesis of C-71
Under a stream of nitrogen AzC-15 (3.0 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 71-C (2.8 g, 62% yield).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
76 Synthesis of C-76
Under a stream of nitrogen AzC-16 (2.6 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 76-C (2.6 g, 64% yield)
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
81 Synthesis of C-81
Under a stream of nitrogen AzC-17 (3.2 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . The reaction was terminated by the filter after the solid salts then purified by column chromatography the desired compound 81-C (3.3 g, yield 70%) was obtained
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
86 Synthesis of C-86
Under a stream of nitrogen AzC-18 (2.4 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210 . After the reaction was terminated to obtain a filter after the solid salt was purified by column chromatography the desired compound 86-C (2.6 g, 65% yield).
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
91 Synthesis of C-91
Under a stream of nitrogen AzC-19 (2.9 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . After the reaction was terminated after filter the solid salt was purified by column chromatography to give the title compound 91-C (3.0 g, yield 67%)
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
96 Synthesis of C-96
Under a stream of nitrogen AzC-20 (3.5 g, 6.7 mmol), 4-bromo-2 ,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), the mixture Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and stirred for 3 hours at 210°C . The reaction was terminated by the filter after the solid salts then purified by column chromatography to give the objective compound C-96 (3.1 g, yield: 61%)
Stage #1: 6-bromo-2,4-diphenyl-pyrimidine With n-butyllithium In diethyl ether; hexane at -78℃; for 0.5h;
Stage #2: Triisopropyl borate In diethyl ether; hexane at -78 - 20℃;
1.2 Sub1-1 (12) Synthesis
Sub 1-1-1 (12) (6.2g, 20mmol) dissolved in anhydrous Ether, a reaction temperatureof -78 ° C to a lower, n-BuLi (2.5M in hexane) (1.4g, 22mmol) was slowly addeddropwise and after I, the reaction is stirred for 30 min. After the dropwise additionTriisopropyl borate (5.64g, 30mmol) lowering the temperature of the reaction back to -78 ° C. Stirring at room temperature, diluted with water and it binds the 2N HCl. Aftercompletion of reaction, the organic layer was dried and extracted with water and ethylacetate over MgSO4 silicagel column and re-crystallization and the resulting organicsconcentrated to give 4g then the Sub 1-1 (12). (Yield: 72%)
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
109 Synthesis of B-1
Under a nitrogen flow AzC-1 (3.7 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound B-1 the for purifying column chromatography (3.5 g, yield 66%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
114 Synthesis of B-6
Under a nitrogen flow AzC-2 (2 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound B-6 the for purifying column chromatography (3.5 g, yield 66%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
119 Synthesis of C-1
Under a nitrogen flow AzC-3 (3.6 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound C-1 the for purifying column chromatography (3.3 g, yield 63%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
124 Synthesis of D-1
Under a nitrogen flow AzC-4 (3.7 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound D-1 the for purifying column chromatography (3.2 g, yield 61%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
129 Synthesis of E-1
Under a nitrogen flow AzC-5 (2.0 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound E-1 the for purifying column chromatography (3.3 g, yield 65%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
134 Synthesis of F-1
Under a nitrogen flow AzC-6 (3.6 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound F-1 the for purifying column chromatography (3.3 g, yield 64%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
139 Synthesis of G-1
Under a nitrogen flow AzC-7 (4 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound G-1 the for purifying column chromatography (3.9 g, yield 71%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
144 Synthesis of H-1
Under a nitrogen flow AzC-8 (4 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound G-1 the for purifying column chromatography (3.6 g, yield 64%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
149 Synthesis of I-1
Under a nitrogen flow AzC-9 (3.5 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound I-1 the for purifying column chromatography (3.2 g, yield 63%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
154 Synthesis of J-1
Under a nitrogen flow AzC-10 (3.2 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound J-1 the for purifying column chromatography (3.0 g, yield 64%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
159 Synthesis of K-1
Under a nitrogen flow AzC-11 (3.0 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound J-1 the for purifying column chromatography (3.0 g, yield 67%)is obtained.
With copper(l) iodide; 1,10-Phenanthroline; caesium carbonate In nitrobenzene at 210℃; for 3h; Inert atmosphere;
164 Synthesis of L-1
Under a nitrogen flow AzC-12 (3.1 g, 6.7 mmol), 4-bromo-2,6-diphenylpyrimidine (2.5 g, 8.0 mmol), CuI (0.13g, 0.67 mmol), 1,10-phenanthroline (0.24 g, 1.34 mmol), Cs2CO3 (4.37 g, 13.4 mmol), and nitrobenzene (25ml) and the mixture was stirred at 210°C for 3 hours.After reaction being terminated after filter solid salt, thereby, a desired compound J-1 the for purifying column chromatography (2.9 g, yield 63%)is obtained.
With tris-(dibenzylideneacetone)dipalladium(0); triphenylphosphine; sodium t-butanolate In toluene at 100℃; for 24h;
II.2.4 (4) Synthesis of Product 2-17
Sub 5 (2) (16g, 5mmol) and Sub 6 (12) (1.7g, 5.5mmol) in toluene and the mixture Pd2(dba)3 (0.2g, 0.25mmol), PPh3 (0.13g, 0.5mmol), NaOt -Bu (132.4g, 15mmol) were madded to each respectively, and refluxed under stirring for 24 hours at 100 °C . drying the organic layer with water and extracted with ether over MgSO4, and the resulting organics concentrated and silicagel column and recrystallized to obtain 1.9g of 2-17. (Yield 71%)
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