Pantethine

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 1.0 g of D-pantethine, 5 ml of 2,2-dimethoxypropane, 5 drops of trifluoroacetic acid and 5 ml of acetone was stirred for 2 days and then evaporated. The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)], giving 1.0 g of the desired compound as a white hygroscopic foam. evaporated The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)]

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 1.0 g of D-pantethine, 5 ml of 2,2-dimethoxypropane, 5 drops of trifluoroacetic acid and 5 ml of acetone was stirred for 2 days and then evaporated. The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)], giving 1.0 g of the desired compound as a white hygroscopic foam. evaporated The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)]

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 1.0 g of D-pantethine, 5 ml of 2,2-dimethoxypropane, 5 drops of trifluoroacetic acid and 5 ml of acetone was stirred for 2 days and then evaporated. The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)], giving 1.0 g of the desired compound as a white hygroscopic foam. evaporated The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)]

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 1.0 g of D-pantethine, 5 ml of 2,2-dimethoxypropane, 5 drops of trifluoroacetic acid and 5 ml of acetone was stirred for 2 days and then evaporated. The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)], giving 1.0 g of the desired compound as a white hygroscopic foam. evaporated The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)]

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 11.9g. of calcium pantothenate, 6.8g. of cystamine dihydrochloride and 7.7g. of 1-hydroxylbenzotrizole were dissolved in 50ml. of pyridine and 10ml. of water, and thereafter pyridine (25ml.) solution of 10.5g. of dicyclohexylcarbodiimide was added thereto at a time, and the reaction was effected at a temperature below 10° C for 1 hour and then for 5 hours at a room temperature. Next the solvent was removed under a reduced pressure, the residue thereof was added with 50ml. of water, and the deposited crystals were removed by filtration. Pyridine left in the filtered mother liquor was completely removed azetropically with water. The residue thereof was added with 50ml. of water and after cooling, the deposited crystals were filtration removed and extracted with 20ml. of chloroform two times. The water layer was treated under a reduced pressure to remove the remaining chloroform, and thereafter like Example 1, passed through the ion exchange resin, and the flowed out liquid was concentrated under a reduced pressure and thereby colorless transparent viscous liquid of pantethine which was the objective compound was obtained. Drying was carried out by means of a vacuum dryer for one night and as a result 9.6g. of pantethine (yield rate 69.2%) was obtained. of 1-hydroxylbenzotrizole were dissolved in 50ml for 5 hours at a room temperature Next the solvent was removed under a reduced pressure the residue thereof was added with 50ml of water, and the deposited crystals were removed by filtration Pyridine left in the filtered mother liquor was completely removed azetropically with water The residue thereof was added with 50ml of water and after cooling filtration removed extracted with 20ml The water layer was treated under a reduced pressure to remove the remaining chloroform was concentrated under a reduced pressure was obtained Drying was carried out by means of a vacuum dryer for one night and as a result 9.6g

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 11.9g. of calcium pantothenate, 5.6g. of cystamine dihydrocloride and 7.7g. of 1-hydroxybenzotriazole were dissolved in a mixed solvent of 50ml. of pyridine, 10ml. of water and 25ml. of benzene, and thereafter pyridine (25ml.) solution of 10.5g. of dicyclohexylcarbodiimide was added thereto at a time, and then this was subjected to reaction at a temperature below 10° C for 1 hour and thereafter to reaction at a room temperature for 5 hours. Then the solvent was removed at a reduced pressure, and the residue thereof was added with 50ml. of water and the resultant deposited crystals were removed by filtration. Pyridine left in the filtered mother liquor was completely removed azeotropically with water. The residue thereof was added with 50ml. of water, and after cooling it, the deposited crystals was removed by filtration, and extracted two times with 20ml. of chloroform. The water layer was passed through a monobed column composed of 78ml. of strong acidic cation exchanger resin (Amberlite 1R-120B) [H+] and 150ml. of strong basic anion exchanger resin (Amberlite 1RA-410) [OH-], and washed out with water. The presence of the objective compound in the flowed out liquid was traced by refractometer. The eluted solution was concentrated under a reduced pressure and subjected to freeze drying, and thereby 9.6g. of pantethine in the form of pulverized crystal was obtained (69.2% yield). at a time, and then this was subjected to reaction at a temperature below 10° C for 1 hour to reaction at a room temperature for 5 hours Then the solvent was removed at a reduced pressure the residue thereof was added with 50ml were removed by filtration Pyridine left in the filtered mother liquor was completely removed azeotropically with water The residue thereof was added with 50ml of water, and after cooling it the deposited crystals was removed by filtration extracted two times with 20ml of strong basic anion exchanger resin (Amberlite 1RA-410) [OH-], and washed out with water The eluted solution was concentrated under a reduced pressure to freeze drying

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 1.0 g of D-pantethine, 5 ml of 2,2-dimethoxypropane, 5 drops of trifluoroacetic acid and 5 ml of acetone was stirred for 2 days and then evaporated. The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)], giving 1.0 g of the desired compound as a white hygroscopic foam. evaporated The resulting white foam was purified by flash chromatography [dichloromethane:methanol (10:1)]