tert-Butyl bromoacetate → HCID 131714545, 화합물
반응식
[O-:1][C:2]#[N:3].[K+].Br[CH2:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8].[C:14]([O:18][C:19]([NH:21][C@H:22]1[C@@H:25]([CH3:26])[NH:24][C:23]1=[O:27])=[O:20])([CH3:17])([CH3:16])[CH3:15]>CN(C)C=O>[C:14]([O:18][C:19]([NH:21][C@H:22]1[C@@H:25]([CH3:26])[N:24]([C:2]([NH:3][CH2:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])=[O:1])[C:23]1=[O:27])=[O:20])([CH3:17])([CH3:15])[CH3:16]참가 물질
반응 조건
- 온도
- 100 °C
실험 절차
To a suspension of potassium cyanate (558 mg, 6.9 mmol) in 6 ml of dimethylformamide was added t-butyl bromoacetate (1.1 ml, 6.6 mmol). The mixture was heated to 100° C. for 1 hour and cooled to room temperature. (3s-cis)-3-[[(t-butyloxy)carbonyl]amino]-4-methyl-2-azetidinone (1.2 g, 6.0 mmol) was then added, and the mixture was heated to 65° C. After being stirred at 65° C. for 1 hour, the mixture was heated to 100° C. and stirred for an additional hour. Additional isocyanate was prepared (using 558 mg potassium cyanate and 1.1 ml of t-butyl bromoacetate as described above) and added to the reaction mixture at room temperature. After being heated at 65° C. for 1 hour and 100° C. for 1 hour, the reaction mixture was stirred at room temperature overnight.
후처리
- temperaturecooled to room temperature
- temperaturethe mixture was heated to 65° C
- temperaturethe mixture was heated to 100° C.
- stirringstirred for an additional hour
- additionadded to the reaction mixture at room temperature
- temperatureAfter being heated at 65° C. for 1 hour and 100° C. for 1 hour
- stirringthe reaction mixture was stirred at room temperature overnight
출처 및 근거
- ORD 기록
- ord-593f1d36d3b746b7947d6c320d5702f0
- 출처 데이터셋
- uspto-grants-1986_03
- 특허 번호
- US04576749
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