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2-{1-[(Tert-butoxycarbonyl)amino]cyclopropyl}ethyl methanesulfonate → HCID 12993141, 화합물

HRID 1786162
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HRID 1786162 반응식
CS(O[CH2:6][CH2:7][C:8]1([NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:10][CH2:9]1)(=O)=O.[C:19]1(=[O:29])[NH:23][C:22](=[O:24])[C:21]2=[CH:25][CH:26]=[CH:27][CH:28]=[C:20]12.[K]>CN(C)C=O>[O:24]=[C:22]1[C:21]2[C:20](=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:19](=[O:29])[N:23]1[CH2:6][CH2:7][C:8]1([NH:11][C:12](=[O:13])[O:14][C:15]([CH3:18])([CH3:17])[CH3:16])[CH2:10][CH2:9]1
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참가 물질

4

반응물 2

HCID 129931402-{1-[(Tert-butoxycarbonyl)amino]cyclopropyl}ethyl methanesulfonateHCID 24194345Phthalimide potassium salt

생성물 1

HCID 12993141HCID 12993141, 화합물수율 50.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

To a solution of 7.82 g (28 mmol) of 2-{1-[(tert-butoxycarbonyl)amino]-cyclopropyl}ethyl methanesulfonate in 35 ml of anhydrous dimethylformamide was added 5.45 g (29.4 mmol) of potassium phthalimide. The resulting mixture was stirred at 150° C. for 18 h. The mixture was then filtered and washed with diethyl ether. The filtrate was evaporated to dryness, the crude product was heated in water and the precipitate was filtered. The product was dried to give 4.63 g of pure compound as an orange solid. Mp: 125-127° C.

후처리

  1. filtrationThe mixture was then filtered
  2. washwashed with diethyl ether
  3. customThe filtrate was evaporated to dryness
  4. temperaturethe crude product was heated in water
  5. filtrationthe precipitate was filtered
  6. customThe product was dried

출처 및 근거

ORD 기록
ord-6b11e0e4e9fa49aabf72bc36725928b3
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07507743B2

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