Sulfuric Acid → HCID 20451897、化合物
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]#[N:10])=[CH:4][C:3]=1[NH2:11].S(=O)(=O)(O)[OH:13].[OH-].[Na+]>O>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=[O:13])[NH2:10])=[CH:4][C:3]=1[NH2:11]参加物
5
実験手順
To 1.03 g. of 1,2-diamino-4-cyanomethylbenzene (1.03 g.) was slowly added concentrated sulphuric acid (7 ml.). The mixture was heated at 90° for 90 minutes, then poured onto 50 ml. of water and ice and adjusted to pH 8 with NaOH. The precipitate which formed on cooling was discarded and the aqueous phase was concentrated to drynes. The residue was extracted with acetone, the extracts were concentrated and chromatographed on silica gel using CH2Cl2 /MeOH 9:1 to 8:2 v/v to give 1,2-diamino-4-carbamoylmethylbenzene (0.65 g.) which was used without further purification.
後処理
- temperatureThe mixture was heated at 90° for 90 minutes
- additionpoured onto 50 ml
- customThe precipitate which formed
- temperatureon cooling
- concentrationthe aqueous phase was concentrated to drynes
- extractionThe residue was extracted with acetone
- concentrationthe extracts were concentrated
- customchromatographed on silica gel
出典と根拠
- ORDレコード
- ord-c3ff2f557df14504940415bd5b70f12f
- 出典データセット
- uspto-grants-1984_07
- 特許番号
- US04463173
反応ノート
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