O-Phenylenediamine → HCID 22139864、化合物
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH2:8].[Cl:9][C:10]1[C:11]([N:15]=[C:16]=[S:17])=[CH:12][S:13][CH:14]=1>C1COCC1>[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:16]([NH:15][C:11]1[C:10]([Cl:9])=[CH:14][S:13][CH:12]=1)=[S:17]参加物
4
実験手順
0.86 g of 1,2-diaminobenzene (o-phenylenediamine) is added to a solution of 1.4 g of 4-chloro-3-thienyl isothiocyanate in 40 ml of anhydrous THF, the mixture is stirred at room temperature for about 20 hours and the solvent is distilled off under reduced pressure. The residue is treated with water and extracted with ethyl acetate, the solvent is distilled off again and the residue is purified using medium-pressure silica gel column chromatography using a 1:1 mixture of ethyl acetate and toluene. Brown-yellow solid.
後処理
- distillationthe solvent is distilled off under reduced pressure
- additionThe residue is treated with water
- extractionextracted with ethyl acetate
- distillationthe solvent is distilled off again
- customthe residue is purified
- additiona 1:1 mixture of ethyl acetate and toluene
出典と根拠
- ORDレコード
- ord-c2a8fb043c9047be92ab89241a938d1b
- 出典データセット
- uspto-grants-2008_01
- 特許番号
- US07317033B2
反応ノート
読み込み中…