Hydrochloric Acid → Urea, (2-hydroxy-4-methylphenyl)-
反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:9])=[CH:6][C:7]=1[OH:8].[NH2:10][C:11](N)=[O:12].Cl>O.C(O)(=O)C>[OH:8][C:7]1[CH:6]=[C:5]([CH3:9])[CH:4]=[CH:3][C:2]=1[NH:1][C:11]([NH2:10])=[O:12]参加物
6
実験手順
To 13 ml of water, there were added 5.00 g (40.7 mmol) of 6-amino-m-cresol, 9.76 g of (162.6 mmol) of urea, 4 ml of conc. hydrochloric acid and 0.8 ml of a mixture (1:1 (v:v)) of conc. hydrochloric acid and glacial acetic acid, followed by heating under reflux for 1.5 hours. After cooling, 20 ml of water was added. The crystals thus precipitated were filtered and dried to thereby give 5.81 g (35.0 mmol) of N-(2-hydroxy-4-methylphenyl)urea as dark brown crystals. The yield was 86%. After recrystallizing from acetonitrile, 2.00 g of N-(2-hydroxy-4-methylphenyl)urea was obtained as pale purple crystals. The recovering yield was 34%.
後処理
- temperatureby heating
- temperatureunder reflux for 1.5 hours
- temperatureAfter cooling
- customThe crystals thus precipitated
- filtrationwere filtered
- customdried
出典と根拠
- ORDレコード
- ord-bf95338779ae475fa9c9bc341d2d4a05
- 出典データセット
- uspto-grants-1994_08
- 特許番号
- US05334225
反応ノート
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