HCID 59625273, 화합물 → HCID 59625433, 화합물

HRID 2192883노트

반응식

HRID 2192883 반응식
[N:1]1([C:5]([C@@H:7]2[CH2:12][C@H:11]([N:13]([C:18]([C:20]3[C:21]([NH:30][CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[N:22][C:23]([C:26]([CH3:29])([CH3:28])[CH3:27])=[N:24][CH:25]=3)=[O:19])[CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8]2)=[O:6])[CH2:4][CH2:3][CH2:2]1>C(OCC)(=O)C.Cl>[N:1]1([C:5]([C@H:7]2[CH2:8][NH:9][CH2:10][C@@H:11]([N:13]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:18]([C:20]3[C:21]([NH:30][CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[N:22][C:23]([C:26]([CH3:28])([CH3:29])[CH3:27])=[N:24][CH:25]=3)=[O:19])[CH2:12]2)=[O:6])[CH2:2][CH2:3][CH2:4]1

참가 물질

3

반응물 1

HCID 59625273HCID 59625273, 화합물

생성물 1

HCID 59625433HCID 59625433, 화합물수율 42.3%

시약·촉매·용매 1

HCID 21866389Hydrogen chloride-ethyl acetate용매

실험 절차

tert-Butyl (3R,5S)-3-(azetidin-1-ylcarbonyl)-5-[({2-tert-butyl-4-[(3-methoxypropyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylate (94 mg) was dissolved in 4 M hydrogen chloride-ethyl acetate (3 ml), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated under reduced pressure, and the residue was subjected to reversed-phase preparative HPLC. Aqueous sodium hydrogen carbonate was added to the object fraction, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the object compound (33 mg).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionAqueous sodium hydrogen carbonate was added to the object fraction
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b2376de9f1784561950b8d58e2acc387
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329691B2

반응 노트

불러오는 중…