Synthesis method of 7-mercaptoisobenzofuran-1(3H)-one compound

[0031] The synthetic method of 7-mercapto-3-methylisobenzofuran-1 (3H)-ketone, the steps are as follows:

[0032] (1) Add compound II and sodium sulfide to DMF, react at 15°C for 5 hours, filter, and evaporate the filtrate to remove the solvent under reduced pressure to obtain a brown solid-liquid mixture;

[0033] Among them, compound II is

[0034] The molar ratio of the compound II and sodium sulfide is 1:1.1;

[0035] (2) Add 30mL water, 30mL methylene chloride and 80wt% acetic acid to the brown solid-liquid mixture gained in step (1), adjust the pH to 5-6, filter, separate liquids, and evaporate the organic solvent under reduced pressure in the organic phase to obtain light Yellow oil, namely 7-mercapto-3-methylisobenzofuran-1(3H)-one; the HPLC area-normalized purity of the product in the reaction solution was 80.71%, and the yield was 82%.

[0036] Analyze the resulting product, 1 H NMR (400MHz, CDCl 3 )δ7.46(t, J=7.7Hz, 1H), 7.28(d, J=7.8Hz, 1H), 7.10(d, J=7.5Hz, 1H)

[0038] The synthetic method of 7-mercapto-3-methylisobenzofuran-1 (3H)-ketone, the steps are as follows:

[0039] (1) Add compound II, sodium sulfide and elemental sulfur to DMF, react at 25°C for 2 hours, filter, and distill the filtrate to remove the solvent under reduced pressure to obtain a brown solid-liquid mixture;

[0040] Among them, compound II is

[0041] The molar ratio of compound II, sodium sulfide and elemental sulfur is 1:1.5:1.65;

[0042] (2) Add 30mL water, 30mL methylene chloride and 80wt% acetic acid to the brown solid-liquid mixture gained in step (1), adjust the pH to be 5-6, filter, separate liquids, and evaporate the organic solvent under reduced pressure in the organic phase to obtain light Yellow oil, namely 7-mercapto-3-methylisobenzofuran-1(3H)-one; the HPLC area-normalized purity of the product in the reaction solution was 88.29%, and the yield was 90%.

[0044] The synthetic method of 7-mercapto-3-methylisobenzofuran-1 (3H)-ketone, the steps are as follows:

[0045] (1) Add compound II, sodium sulfide and elemental sulfur to DMF, react at 0°C for 5 hours, filter, and evaporate the filtrate to remove the solvent under reduced pressure to obtain a brown solid-liquid mixture;

[0046] Among them, compound II is

[0047] The molar ratio of compound II, sodium sulfide and elemental sulfur is 1:1.5:1.65;

[0048] (2) Add 30mL water, 30mL methylene chloride and 80wt% acetic acid to the brown solid-liquid mixture gained in step (1), adjust the pH to be 5-6, filter, separate liquids, and evaporate the organic solvent under reduced pressure in the organic phase to obtain light Yellow oil, namely 7-mercapto-3-methylisobenzofuran-1(3H)-one; the HPLC area-normalized purity of the product in the reaction solution was 80.99%, and the yield was 85%.