628-21-7, name is 1,4-Diiodobutane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C4H8I2
Example 3 (n=4); (a) 1, 1′-[(Butane-1,4-diyl)dioxy]bis[(11S,11aS)-10-(tert- butyloxycarbonyl)-8-methoxy-ll- (tetrahydro-pyran-2-yloxy)- 1, 2,3, 10, 11, 11a-hexahydro-5H-pyrrolo[2,-c][1,4]benzodiazepine-5-one](8b); 1,4-Diiodobutane (69.1 mg, was added to the mixture of monomer 7 (0.2 g, 0.44 mmol, 1.0 equiv) and potassium carbonate (0.98 mmol, 2.2 equiv) in dry DMF (30 mL), and the resulting mixture was heated to 90C under a nitrogen atmosphere for 5 h. Removal of excess solvent under reduced pressure afforded a crude solid, which was subjected to flash column chromatography (SiO2, 50% EtOAc- hexane) to afford the dimerized compound 8b (134 mg, 0.14 mmol, 63% yield, mixture of diastereomers from THP protecting group as a solid: [a] 20D = +36 (c = 0. 19, CHCl3) ; 1H NMR (CDC, 400 MHz): 5 1.35 (s, 36H, Boc), 1.45-1. 67 (m, 16H, THP), 1.68-1. 86 (m, 8H, THP), 1.90-2. 21 (m, 24H, 1-H, 2-H, 13-H), 3.44-3. 78 (m, 16H, 3-H, lla-H, THP), 3.84-4. 02 (m, 16H, 7-OMe, THP), 4. 04-4. 25 (m, 8H, 12- H), 5.02-5. 10 (m, 2H, THP), 5.11-5. 20 (m, 2H, THP), 5.69-5. 77 (d, 2H, 11-H), 5.79-5. 89 (d, 2H, 11-H), 6.51 (s, 2H, 9-H), 6.88 (s, 2H, 9-H), 7.19 (s, 2H, 6-H), 7.28 (s, 2H, 6-H) ; 13C NMR (CDCl3, 400 MHz): No. 19.8, 20.5, 23.1, 23.2, 25.3, 25.9, 28.1, 28. 2,28. 9, 29.1, 30.9, 31.2, 46.2, 55.9, 56.2, 60.1, 63.3, 63.6, 68.6, 80.9, 88.2, 91.2, 96.2, 100.2, 111.1, 111.4, 113.4, 114.1, 118.5, 126.4, 129.8, 143.1, 147.9, 148.2, 151. 5, 151. 8,155. 8,167. 4,167. 6; IR (neat): 2945,1704, 1644, 1604,1513, 1449,1392, 1327,1217, 1163, 1022cm~1 ; MS (FAB) m/z (relative intensity) 973 ([M + Na] +, 11), 951 (M +, 100), 749 (36).
The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SPIROGEN LIMITED; WO2005/85259; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com