The preparation method of darunavir intermediate
A compound and aromatic ring technology, applied in the direction of organic chemistry, can solve the problems of expensive active reagents and low yield of active esters, and achieve high industrial application and economic value, high reactivity, and simple reaction types.
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Embodiment 1
[0063] Embodiment 1: the preparation of formula 3 compound
[0064]
[0065] Triphosgene (5.86g, 0.02mol) was dissolved in 20ml of dichloromethane, raised to 50°C, (3R, 3aS, 6aR)-hexahydrofuro[2,3-b]furan-3-ol (2.60g, 0.02 mol) and triethylamine (3.00g, 0.0.03mol) were mixed and dissolved in 25ml of dichloromethane, added dropwise to the reactor, after the dropwise addition was completed, the reaction was continued for 3 hours, TLC detected that the raw materials disappeared, and a quantitative crude compound of formula 3 was obtained.
Embodiment 2
[0066] Embodiment 2: the preparation of formula 6-1 compound
[0067]
[0068] The compound of formula 3 (3.8g, 0.02mol) obtained in Example 1 was dissolved in 30ml of tetrahydrofuran, and added dropwise to N-hydroxyl
[0069] Add triethylamine (2.02g, 0.02mol) to a 45ml tetrahydrofuran solution of succinimide (2.3g, 0.02mol), add dropwise, reflux, react for 2 hours, TLC detects that the raw materials disappear, add aqueous solution of salt water to extract , and concentrated the upper layer to obtain 5.4 g of the compound of formula 6-1, with a yield of 99.6%.
Embodiment 3
[0070] Embodiment 3: the preparation of formula 6-2 compound
[0071]
[0072] The compound of formula 3 (3.8g, 0.02mol) obtained in Example 1 was added dropwise in 45ml of dichloromethane solution of N-hydroxyphthalimide (3.26g, 0.02mol), and pyridine (1.58g , 0.02mol) was added dropwise, refluxed, and reacted for 1.5 hours. TLC detected that the raw materials disappeared, added water for liquid extraction, and concentrated the lower layer to obtain 6.3g of the compound of formula 6-2, with a yield of 98.7%.
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