Urea → 1-(p-Tolyl)-3-azabicyclo[3.1.0]hexane-2,4-dione
반응식
[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]=1참가 물질
4
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-1a5375979fb5402d8fe980b291f4b317
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094799B2
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