Water → Sulfanilic acid
反応式
[NH2:1]C1C=C[C:9]2[C:4](=[CH:5][C:6]([S:13]([OH:16])(=[O:15])=[O:14])=[CH:7][C:8]=2O)C=1.[OH-:17].[Na+:18].FC1N=C(F)C=C(F)[N:21]=1.C(=O)([O-])[O-].[Na+].[Na+].[OH2:34]>>[NH2:21][C:9]1[CH:8]=[CH:7][C:6]([S:13]([OH:16])(=[O:15])=[O:14])=[CH:5][CH:4]=1.[N:1]([O-:34])=[O:17].[Na+:18]参加物
反応条件
- 温度
- 42.5 °C
実験手順
47.8 parts of 2-amino-5-hydroxynaphthalene-7-sulfonic acid are stirred into 500 parts of water at 25° C. and are dissolved by the addition of 22 parts of a 30% by weight solution of sodium hydroxide. To this solution is added 26.8 parts of 2,4,6-trifluoropyrimidine dropwise over a 30 minute period. At the same time a 20% of sodium carbonate solution is added to this mixture continuously in order to maintain the pH of the mixture at 4-5. The reaction temperature is increased to 40-45° C. The end point of the reaction is determined using chromatographic techniques. The resultant suspension is cooled to 20-25° C. and poured onto a diazonium salt solution which is formed of 34.6 parts of 4-aminobenzene-sulfonic acid and 50 parts by volume of 4 N sodium nitrite solution at 0-5° C. and a pH of 1. During the coupling reaction the pH is maintained at 6-7 by continuously adding 20% sodium carbonate solution. The monoazo compound thus formed is salted-out using conventional methods, filtered and dried at 60° C. under vacuum. The product has the formula ##STR8##
後処理
- temperatureto maintain the pH of the mixture at 4-5
出典と根拠
- ORDレコード
- ord-eb60c21061aa4b44b73c10feacf3286d
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06127531
反応ノート
読み込み中…