Method for preparing 6-methyl-1,2,3-oxazine-4(3H)-ketone-2,2-dioxopotassium salt
A technology of potassium dioxooxide and oxthiazine is applied in the field of preparing 6-methyl-1, can solve the problems of large product loss, high reaction temperature, short reaction steps and the like, and achieves low cost, simple synthesis and purification yield high effect
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Embodiment 1
[0063] 1. Preparation of acetoacetamidosulfonyl fluoride potassium salt:
[0064] Add 98g (1mol) of potassium acetate to 500ml of acetone, add 99g (1mol) of sulfamoyl fluoride at about 0°C under stirring, then add 84g (1mol) of diketene dropwise within 30 minutes under the same conditions, and continue to Stir at 0°C for 30 minutes, then rise to room temperature and stir at 20-25°C for 4 hours, filter, and wash twice with 40ml of acetone to obtain 200g of white crystalline solid, y=90%. It can be directly used in the next reaction.
[0065] 2. Preparation of crude product of 6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxyl potassium salt
[0066] Add the above acetoacetamidosulfonyl fluoride potassium salt to a solution of 60g KOH in 300ml methanol, stir at room temperature at 20-25°C for 4 hours, filter, and wash with 20ml methanol to obtain 194g of crude product, y=97%.
[0067] 3. Preparation of 6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxopotassium salt
Embodiment 2
[0070] 1. Preparation of acetoacetamidosulfonyl fluoride sodium salt:
[0071] Add 70g (1mol) of sodium acetate to 500ml of acetone, add 99g (1mol) of sulfamoyl fluoride at about 0°C under stirring, then add 84g (1mol) of diketene dropwise within 30 minutes under the same conditions, and continue to Stir at 0°C for 30 minutes, then rise to room temperature and stir at 20-25°C for 4 hours, filter, and wash twice with 40ml of acetone to obtain 200g of white crystalline solid, y=90%. It can be directly used in the next reaction.
[0072] 2. Preparation of crude product of 6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxosodium salt
[0073] Add the above sodium acetoacetamidosulfonyl fluoride to a solution of 60g KOH in 300ml methanol, stir at room temperature at 20-25°C for 4 hours, filter, and wash with 20ml methanol to obtain 194g of crude product, y=97%.
[0074] 3. Preparation of 6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxopotassium salt
[0075] Dissolve 100g of crude acesu...
Embodiment 3
[0077] Prepare 6-methyl-1,2,3-oxathiazin-4(3H)-ketone-2,2-dioxo potassium salt by the method of Example 1, just replace the potassium succinate in Example 1 potassium acetate.
[0078] 1. Preparation of acetoacetamidosulfonyl fluoride potassium salt:
[0079] Add 194g (1 equivalent) of potassium succinate to 500ml of acetone, add 99g (1mol) of sulfamoyl fluoride at about 0°C under stirring, then add 84g (1mol) of diketene dropwise within 30 minutes under the same conditions, and add Continue to stir at 0°C for 30 minutes, then rise to room temperature and stir at 20-25°C for 4 hours, filter, and wash twice with 40ml of acetone to obtain 190g of white crystalline solid, y=85%. It can be directly used in the next reaction.
[0080] 2. Preparation of crude product of 6-methyl-1,2,3-oxathiazin-4(3H)-one-2,2-dioxyl potassium salt
[0081] The above-mentioned acetoacetamidosulfonyl fluoride potassium salt was added to a solution of 60g KOH in 300ml methanol, stirred at room tempe...
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