反応式
S(=O)(=O)(O)O.[C:6]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)#[N:7].[CH2:14]=[C:15]([CH3:17])[CH3:16].[OH-:18].[Na+]>C(O)(=O)C>[C:15]([NH:7][C:6]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)=[O:18])([CH3:17])([CH3:16])[CH3:14]参加物
実験手順
575 g (5.75 mmol) of sulfuric acid was added dropwise to 900 ml of acetic acid over 35 minutes at 20° C. (cooling), followed by 200.1 g (1.9 mol) of cyanopyrazine over 20 minutes. 142.4 g (2.54 mol) of isobutene was then introduced over 3.5 hours, the temperature being kept below 25° C. by appropriate cooling. The mixture was subsequently stirred for a further 2 hours at room temperature and then poured into 1.8 l of ice-water. The mixture was brought to pH 3.5 by the slow addition of 1527 g of 30 percent sodium hydroxide solution and then extracted continuously for 4 hours with 2.5 l of hot methylcyclohexane in a liquid-liquid extractor. The extract was cooled to 4° C., with stirring, and the product which had crystallized out was filtered off and dried under vacuum. The yield of the title compound was 246 g, content (titration): 99.6 percent. Concentration of the mother liquor gave a further 22.5 g of the title compound with a content of 99.0 percent. The total yield of the title compound was 268.5 g (78 percent).
後処理
- temperature(cooling)
- custombeing kept below 25° C. by appropriate cooling
- extractionextracted continuously for 4 hours with 2.5 l of hot methylcyclohexane in a liquid-liquid extractor
- temperatureThe extract was cooled to 4° C.
- stirringwith stirring
- customthe product which had crystallized out
- filtrationwas filtered off
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-1ca05b56705d4c00a30c9ff1bfe4645a
- 出典データセット
- uspto-grants-1999_08
- 特許番号
- US05945534
関連ノート
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