* 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.
With caesium carbonate; In N,N-dimethyl-formamide; at 20℃;
Example 144; 5-[4-(6-Fluoro-benzothiazol-2-yloxy)-benzyl]-hexahydro-pyrrolo[3,4-c]pyrrole-2-carboxylic acid amideStep A: [4-(6-Fluoro-benzothiazol-2-yloxy)-phenyl]-methanol. A mixture of <strong>[154327-27-2]2-chloro-5-fluorobenzthiazole</strong> (2.2 g, 12.0 mmol), 4-hydroxylbenzyl alcohol (1.48 g, 12.0 mmol) and Cs2CO3 (8.6 g, 26.4 mmol) in DMF (30 mL) was stirred at rt overnight. The reaction was filtered and diluted with CH2Cl2 (200 mL) and concentrated. The crude mixture was purified via silica gel column chromatography (1% to 15% CH3OH/CH2Cl2) to afford the title compound (1.1 g, 34%). MS (ESI): Mass calcd for C14H10NO2SF, 275.0; m/z found, 276.1 [M+H]+
With hydrogenchloride; In water; for 0.25h;pH 5.25;
General procedure: Proper amount of fresh RGE slices were ground in a mortar. The pH value of fresh RGE juicewas 5.25 measured by pH meter. The above 10 monomer compounds were precisely weighed 1.0 mg, dissolved by 1.0 mL hydrochloric acid solution of pH 5.25, and placed in a vial. The sample solution of 1.0 mg/mL was obtained. The vials of 10 samples were steamed in the steamer simulating the steaming process of RGE. The timing started after the round vapor. After 15 min, the vials were taken out. After cooling to room temperature, the analysis was carried out under the condition of Section 3.5, PA was analyzed by HPLC-ESI-TOF/MS and the other nine compounds were analyzed by HPLC.
3-hydroxy-5-oxo-5-[[4-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyphenyl]methoxy]-3-[[4-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyphenyl]methoxycarbonyl]pentanoic acid[ No CAS ]
[ 623-05-2 ]
[ 952068-57-4 ]
[ 952283-93-1 ]
[ 62499-27-8 ]
Yield
Reaction Conditions
Operation in experiment
With hydrogenchloride; In water; for 0.25h;pH 5.25;
General procedure: Proper amount of fresh RGE slices were ground in a mortar. The pH value of fresh RGE juicewas 5.25 measured by pH meter. The above 10 monomer compounds were precisely weighed 1.0 mg, dissolved by 1.0 mL hydrochloric acid solution of pH 5.25, and placed in a vial. The sample solution of 1.0 mg/mL was obtained. The vials of 10 samples were steamed in the steamer simulating the steaming process of RGE. The timing started after the round vapor. After 15 min, the vials were taken out. After cooling to room temperature, the analysis was carried out under the condition of Section 3.5, PA was analyzed by HPLC-ESI-TOF/MS and the other nine compounds were analyzed by HPLC.
With hydrogenchloride; In water; for 0.25h;pH 5.25;
General procedure: Proper amount of fresh RGE slices were ground in a mortar. The pH value of fresh RGE juicewas 5.25 measured by pH meter. The above 10 monomer compounds were precisely weighed 1.0 mg, dissolved by 1.0 mL hydrochloric acid solution of pH 5.25, and placed in a vial. The sample solution of 1.0 mg/mL was obtained. The vials of 10 samples were steamed in the steamer simulating the steaming process of RGE. The timing started after the round vapor. After 15 min, the vials were taken out. After cooling to room temperature, the analysis was carried out under the condition of Section 3.5, PA was analyzed by HPLC-ESI-TOF/MS and the other nine compounds were analyzed by HPLC.
3-hydroxy-5-oxo-5-[[4-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyphenyl]methoxy]-3-[[4-[(2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyphenyl]methoxycarbonyl]pentanoic acid[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With hydrogenchloride; In water; for 0.25h;pH 5.25;
General procedure: Proper amount of fresh RGE slices were ground in a mortar. The pH value of fresh RGE juicewas 5.25 measured by pH meter. The above 10 monomer compounds were precisely weighed 1.0 mg, dissolved by 1.0 mL hydrochloric acid solution of pH 5.25, and placed in a vial. The sample solution of 1.0 mg/mL was obtained. The vials of 10 samples were steamed in the steamer simulating the steaming process of RGE. The timing started after the round vapor. After 15 min, the vials were taken out. After cooling to room temperature, the analysis was carried out under the condition of Section 3.5, PA was analyzed by HPLC-ESI-TOF/MS and the other nine compounds were analyzed by HPLC.
With hydrogenchloride; In water; for 0.25h;pH 5.25;
General procedure: Proper amount of fresh RGE slices were ground in a mortar. The pH value of fresh RGE juicewas 5.25 measured by pH meter. The above 10 monomer compounds were precisely weighed 1.0 mg, dissolved by 1.0 mL hydrochloric acid solution of pH 5.25, and placed in a vial. The sample solution of 1.0 mg/mL was obtained. The vials of 10 samples were steamed in the steamer simulating the steaming process of RGE. The timing started after the round vapor. After 15 min, the vials were taken out. After cooling to room temperature, the analysis was carried out under the condition of Section 3.5, PA was analyzed by HPLC-ESI-TOF/MS and the other nine compounds were analyzed by HPLC.
With hydrogenchloride; beta-D-glucosidase; In water; at 35℃; for 2h;pH 5.25;Enzymatic reaction;
GAS (0.591 mg/mL) and beta-D-glucosidase (1.24 mg/mL) were dissolved in hydrochloric acidsolution of pH 5.25 in a vial. Two copies of the above samples were prepared. One was steamed on a steamer for 15 min, and the other was incubated in water bath at 35 C for 2 h. A 10 L aliquot was injected for HPLC analysis.
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