2265-91-0, name is 1,3-Difluoro-5-iodobenzene, 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. Application In Synthesis of 1,3-Difluoro-5-iodobenzene
General procedure: In a microwave tube, 425 mg of (S)-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one (Example 1e) are introduced into 1 ml of dimethylformamide, 422 mg of tripotassium phosphate, 380 mg of copper iodide and 2 ml of iodobenzene. The mixture obtained is heated in a microwave oven for 30 minutes at 150 C. The reaction mixture is then centrifuged. The separated supernatant is then rinsed with ethyl acetate and then evaporated to dryness. The residue is taken up with ethyl acetate and the solution obtained is washed with water. The organic phase is separated and then dried over magnesium sulphate, filtered, and concentrated under vacuum. After purification by silica chromatography (gradient of 5% to 15% of the eluent CH2Cl2/MeOH/NH4OH 28% 38/17/2 in dichloromethane), 150 mg of (8S)-2-(morpholin-4-yl)-9-phenyl-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one are obtained The product is prepared according to the procedure described in Example 12, but using 250 mg of (8S)-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one (Example 1e), 276 mg of 1,3-difluoro-5-iodobenzene, 349 mg of tripotassium phosphate, 156 mg of copper iodide and 93 mg of (1S,2S)-cyclohexane-1,2-diamine. After 1 hour at 150 C. under microwave irradiation and silica column purification of the reaction mixture (elution gradient of CH2Cl2 to CH2Cl2/MeOH 98/02), 91 mg of (8S)-9-(3,5-difluorophenyl)-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetra-hydro-4 H-pyrimido[1,2-a]pyrimidin-4-one are obtained in the form of an ochre foam
The synthetic route of 2265-91-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Sanofi; Baku, Eritsuku; Bulolo, Morice; Cross, Annie; El Amado, Youssef; Fuiroshiyu, Lom Brunnow; Array, Frank; Carlson, Carl Andreas; Marciniak, Gilbert; Ronan, Baptiste; Shio, Laulan; Bibe, Bertrand; Viviani, Fabrice; Zimerman, Andre; (90 pag.)JP5655070; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com