Urea → 1-(p-Tolyl)-3-azabicyclo[3.1.0]hexane-2,4-dione
反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:14]([OH:16])=O)[CH2:10][CH:9]2[C:11](O)=[O:12])=[CH:4][CH:3]=1.[NH2:17]C(N)=O>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]23[CH2:10][CH:9]2[C:11](=[O:12])[NH:17][C:14]3=[O:16])=[CH:4][CH:3]=1参加物
4
実験手順
A mixture of purified 1-(4-methylphenyl)-1,2-cyclopropanedicarboxylic acid (58 kg), toluene (465 kg) and urea (23.8 kg) was heated to reflux and the mixture held at reflux until the reaction was complete. On completion of the reaction period, the solution was cooled to 80–90° C. and washed with water (69 L). The lower aqueous layer was discarded. In this way (±)-1-(4-methylphenyl)-3-azabicyclo[3.1.0]hexan-2,4-dione was obtained as a solution in toluene.
後処理
- temperaturewas heated
- temperatureto reflux
- temperatureat reflux until the reaction
- customOn completion of the reaction period
- temperaturethe solution was cooled to 80–90° C.
- washwashed with water (69 L)
出典と根拠
- ORDレコード
- ord-1a5375979fb5402d8fe980b291f4b317
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07094799B2
反応ノート
読み込み中…