Silicon carbide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 644 g of a silicon nitride powder (SN-E10 manufactured by Ube Industries, Ltd.; average particle size: 0.3 μm), 276 g of a silicon carbide (beta random ultrafine grade manufactured by Ibiden Co., Ltd.; average particle size: 0.27 μm), 80 g of an yttrium oxide powder (manufactured by Nippon Yttrium Co., Ltd.; average particle size: 1.4 μm) and 1000 g of ethanol as the dispersion medium were blended under pulverizing in a ball mill for 18 hours using 800 g of silicon nitride balls as a tumbling media. The resultant mixture was dried to obtain a starting ceramic powder mixture having a BET specific surface area of 12.1 m2 /g. The above amounts, 644 g of silicon nitride and 276 g of silicon carbide, correspond to theoretical amounts of silicon nitride and silicon carbide formed from 578.6 g of silicon and 82.9 g of carbon black used in Example 1. The resultant mixture was dried to obtain a starting ceramic powder mixture

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 500 cm3 flask, provided with a cooling device, were added successively 21.3 g (0.1 mole) of 2,4,5-trimethoxy nitrobenzene, 80 g of chemically pure stannous chloride for mirror making, 100 cm3 of a hydrochloric acid solution (d=1.18) and carborundum. The mixture was brought to boiling under reflux for 1 h. After cooling, a caustic soda solution was added until the precipitate disolved. The solution obtained was extracted with methylene chloride. The organic extracts were dried over sodium sulfate then evaporated under reduced pressure. The residue obtained was crystallized in ethanol. Into a 500 cm3 flask, provided with a cooling device under reflux for 1 h After cooling The solution obtained was extracted with methylene chloride The organic extracts were dried over sodium sulfate then evaporated under reduced pressure The residue obtained was crystallized in ethanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a two liter flask, provided with a cooling device, were introduced successively a solution of methanolic potash (100 g of KOH and 500 cm3 of methanol), then 100 g (0.46 mole) of 4,5-dimethoxy 2-nitro chlorobenzene and carborundum. The mixture was brought to boiling under reflux for 6 h. After cooling, the reaction medium was filtered; the precipitate obtained was washed with methanol. Into a two liter flask, provided with a cooling device under reflux for 6 h After cooling the reaction medium was filtered the precipitate obtained was washed with methanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a two liter flask, provided with a cooling device, were introduced successively a solution of methanolic potash (100 g of KOH and 500 cm3 of methanol), then 100 g (0.46 mole) of 4,5-dimethoxy 2-nitro chlorobenzene and carborundum. The mixture was brought to boiling under reflux for 6 h. After cooling, the reaction medium was filtered; the precipitate obtained was washed with methanol. Into a two liter flask, provided with a cooling device under reflux for 6 h After cooling the reaction medium was filtered the precipitate obtained was washed with methanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Dioscorea deltoides (Mexican yam) cells (about 300-400 mg. fresh weight per flask) were grown in the dark in suspension in a growth medium, as described by Murashige and Skook (Physiol. Plantarum 1962 15: 473), containing 0.1 mg./l. 2,4-dichlorophenoxyacetic acid, 1 mg./l. nicotinic acid, 10 mg./l. thiamine-HCl, 1 mg./l. pyridoxine-HCl and 100 mg./l. inositol, in 125 ml. Erlenmeyer flasks on a rotary shaker (100 rpm, 28° C.). The volume of growth medium per flask was 30 ml., which contained about 10-20 mg. fine mesh carborundum and about 10 mg. sodium orthovanadate. An approximately equimolar amount of sodium metavanadate could be used instead of the orthovanadate. Comparative runs were carried out with and without addition to the medium of elicitor in the form of oxidized BSA (20 μg./ml.). After about 3 weeks, the cells were harvested, lyophilized, refluxed for 2 hours in 2N HCl, filtered, washed with water and dried. The cells were then extracted with chloroform at 60° C., the extract was filtered and evaporated to dryness, and the residue was taken up in chloroform and chromatographed. The spots were visualized with antimony chloride in chloroform. The spots were then dissolved in chloroform and the O.D. read in a spectrophotometer. Some determinations were made by GLC. In absence of elicitor there were obtained 0.1% (dry weight) diosgenin, compared with 3.8% (dry weight) in presence of elicitor, the latter representing a 38 fold enhancement of yield. The dry weight of cells at the end of the run was 1.6 g. per flask. containing 0.1 mg on a rotary shaker (100 rpm, 28° C.) The volume of growth medium per flask was without addition to the medium of elicitor in the form of oxidized BSA (20 μg./ml.) After about 3 weeks filtered washed with water dried The cells were then extracted with chloroform at 60° C. the extract was filtered evaporated to dryness chromatographed The spots were then dissolved in chloroform

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Nicotiana tabacum cv. Xanthi (tobacco) leaf cells (about 300-400 mg. fresh weight per flask) were grown in the dark in suspension in a growth medium, as described by Murashige and Skook (Physiol. Plantarum 1962 15: 473), containing 1 mg./l. 1-naphthaleneacetic acid, 0.1 mg./l. kinetin and 3% sucrose in 125 ml. Erlenmeyer flasks on a rotary shaker (120 rpm, 25° C.). The volume of growth medium per flask was 30 ml., which contained about 10-20 mg. fine mesh carborundum. Comparative runs were carried out with and without addition to the medium of modified protein in the form of oxidized BSA (20 μg./ml.). After 4 weeks, the cells were harvested, weighted, frozen and lyophilized. The dried cells were extracted with methanol in a Soxhlet extractor and the extract was evaporated to dryness at 40° C. with a Buchi Rotoevaporator. The residue was dissolved in 0.5N HCl and extracted with ether. The aqueous layer was brought to pH 9.5 with NaOH, extracted twice with ether and the combined two ether extracts were dried with K2CO3, prior to adding HCl and then evaporating to dryness. The residue was dissolved in 0.5N HCl and aliquots were applied to TLC plates of silica gel G (Merck). The plates were developed in 85:14:1 chloroform-ethanol-ammonia, dried in a stream of N2, and alkaloids were visualized by Dragendorff's reagent. Quantitatively the alkaloids were determined by GLC analysis. In absence of elicitor there were obtained 2.8×10-3 % (dry weight) nicotine, compared with 2.2% (dry weight) in presence of elicitor, the latter representing a 7.8×103 fold enhancement of yield. The dry weight of cells at the end of the run was 3.2 g. per flask. containing 1 mg on a rotary shaker (120 rpm, 25° C.) The volume of growth medium per flask was without addition to the medium of modified protein in the form of oxidized BSA (20 μg./ml.) After 4 weeks weighted, frozen The dried cells were extracted with methanol in a Soxhlet extractor the extract was evaporated to dryness at 40° C. with a Buchi Rotoevaporator The residue was dissolved in 0.5N HCl extracted with ether extracted twice with ether were dried with K2CO3 to adding HCl evaporating to dryness The residue was dissolved in 0.5N HCl dried in a stream of N2, and alkaloids

反応条件: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2,6-dichloro-3-nitro-pyridine (2.5 g, 12.9 mmol) is taken up in a solvent mixture of THF and NMP (5:1, 13 mL), combined with two spatula tips of silicon carbide and CuCN (2.3 g, 26.0 mmol) and heated to 180° C. in the microwave reactor for 45 min. Then the solid obtained is suspended in H2O, extracted with ethyl acetate, washed with NaCl-sln., the organic phase is dried on MgSO4, the solvent is eliminated in vacuo and 6-chloro-3-nitro-pyridine-2-carbonitrile (HPLC-MS: tRet.=1.01 min, MS(M+H)+=182, method LCMSBAS1) is obtained. Then the solid obtained extracted with ethyl acetate washed with NaCl-sln , the organic phase is dried on MgSO4

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 644 g of a silicon nitride powder (SN-E10 manufactured by Ube Industries, Ltd.; average particle size: 0.3 μm), 276 g of a silicon carbide (beta random ultrafine grade manufactured by Ibiden Co., Ltd.; average particle size: 0.27 μm), 80 g of an yttrium oxide powder (manufactured by Nippon Yttrium Co., Ltd.; average particle size: 1.4 μm) and 1000 g of ethanol as the dispersion medium were blended under pulverizing in a ball mill for 18 hours using 800 g of silicon nitride balls as a tumbling media. The resultant mixture was dried to obtain a starting ceramic powder mixture having a BET specific surface area of 12.1 m2 /g. The above amounts, 644 g of silicon nitride and 276 g of silicon carbide, correspond to theoretical amounts of silicon nitride and silicon carbide formed from 578.6 g of silicon and 82.9 g of carbon black used in Example 1. The resultant mixture was dried to obtain a starting ceramic powder mixture

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 644 g of a silicon nitride powder (SN-E10 manufactured by Ube Industries, Ltd.; average particle size: 0.3 μm), 276 g of a silicon carbide (beta random ultrafine grade manufactured by Ibiden Co., Ltd.; average particle size: 0.27 μm), 80 g of an yttrium oxide powder (manufactured by Nippon Yttrium Co., Ltd.; average particle size: 1.4 μm) and 1000 g of ethanol as the dispersion medium were blended under pulverizing in a ball mill for 18 hours using 800 g of silicon nitride balls as a tumbling media. The resultant mixture was dried to obtain a starting ceramic powder mixture having a BET specific surface area of 12.1 m2 /g. The above amounts, 644 g of silicon nitride and 276 g of silicon carbide, correspond to theoretical amounts of silicon nitride and silicon carbide formed from 578.6 g of silicon and 82.9 g of carbon black used in Example 1. The resultant mixture was dried to obtain a starting ceramic powder mixture

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Nitrogen gas was introduced downflow to a 1″×18″ 316 s.s. hot tube reactor system containing 67 ml of silicon carbide (SiC) at a total rate of 6.2 ml/min. The hot tube reactor was heated to 450° C. at which time 1-methoxyoctane (MO), obtained from hydrogenation of 1-methoxy-2,7-octadiene, was added downflow at 0.1 ml/min. Under these conditions 1-methoxyoctane was converted to a mixture of 1-octene and mixed internal octenes at 3.3% wt conversion with a selectivity to 1-octene of 10 m % and mixed internal octenes of 90 m %. Nitrogen gas was introduced downflow to a 1″×18″ 316 s

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Nitrogen gas was introduced downflow to a 1″×18″ 316 s.s. hot tube reactor system containing 67 ml of silicon carbide (SiC) at a total rate of 6.2 ml/min. The hot tube reactor was heated to 450° C. at which time 1-methoxyoctane (MO), obtained from hydrogenation of 1-methoxy-2,7-octadiene, was added downflow at 0.1 ml/min. Under these conditions 1-methoxyoctane was converted to a mixture of 1-octene and mixed internal octenes at 3.3% wt conversion with a selectivity to 1-octene of 10 m % and mixed internal octenes of 90 m %. Nitrogen gas was introduced downflow to a 1″×18″ 316 s