* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Multi-step reaction with 3 steps
1.1: triethylamine; trichlorophosphate / tetrahydrofuran / 3 h / 0 °C
2.1: triethylamine / tetrahydrofuran / 1 h / 40 °C
3.1: acetic acid / methanol / 15 h / 25 °C
3.2: 1 h / 25 °C
Multi-step reaction with 3 steps
1: 1,8-diazabicyclo[5.4.0]undec-7-ene / toluene / 0 - 30 °C
2: boron trifluoride diethyl etherate / toluene / 0 - 30 °C
3: trimethylsilyl iodide / toluene / -10 - 20 °C
Stage #1: C45H87O10P With acetic acid In methanol at 25℃; for 15h;
Stage #2: With sodium carbonate In tetrahydrofuran; water at 25℃; for 1h;
2.4 The preparation of compound phosphatidylglycerol monosodium salt [R=CH3(CH2)14]
To a 50 ml single-necked flask was added 2.0 g of the starting material (compound of formula (III)),20 ml of methanol,6 ml of 30% acetic acid (HOAc),Reaction at room temperature (25 ° C)Reaction for 15 hours,After the reaction,Add 20 ml of ethyl acetate (EA) to dissolve,Organic phase and then water,Salt washed,Dried over sodium sulfate for 24 hours,filter,The solvent is distilled off,Add 20 ml of tetrahydrofuran (THF) to dissolve,Add 2.0 g of Na2CO3 and 20 ml of water,Stirred at room temperature for 1 hour,Filter, dry,A white solid fatty acylglycerol monosodium salt was obtained[R = CH3 (CH2) 14] 1.78 g, yield 91%.
With triethylamine In methanol; chloroform at 20℃; for 24h; Inert atmosphere; Cooling with ice;
7 Example 7 Synthesis of AC-DSPG
Dissolve AC (50 [mu] L, 0.6 mmol) at room temperature using 1 mL of chloroform,And dissolved in 80 mg of chloroform: methanol = 4: 1 DSPG, 26 [mu] L of triethylamine was added.Ice water bath under the conditions of AC chloroform solution gradually added to the DSPG solution, charged N2 protection, Room temperature magnetic stirring reaction 24h. After completion of the reaction, dialysis was performed with 4 volumes of water and dialysis (dialysis bag retention molecular weight)1KDa), the contents of the dialysis bag were freeze-dried to get AC-DSPG. The structure is as follows:
Stage #1: C49H89O10P With trimethylsilyl iodide In toluene at -10 - 20℃;
Stage #2: With sodium methylate In methanol
1.3; 2.3
Weigh out Intermediate 21 10.00g 11.50mmol,Add 100ml of toluene and mix well,Cooled in an ice-salt bath, the temperature of the reaction liquid is controlled at -10-0,Combine 4.60g of trimethylsilyl iodide solution andA solution made of 10ml of toluene was slowly added dropwise to the reaction solution,Control the dripping in 10-20min,Raise the temperature of the reaction solution to 10-20°C,Stir the reaction for 0.5-1.0hr,After the reaction, 5ml of methanol solution containing 0.62g of sodium methoxide was added, a white solid precipitated, filtered and dried.8.16g of white solid is obtained, which is product 1.Yield: 88.54%. Product purity: 97.76%
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
110K+ Compounds
Competitive Price
1-2 Day Shipping
