Hydrochloric Acid → HCID 68420297, 화합물

HRID 20243노트

반응식

HRID 20243 반응식
Cl.[NH2:2][C:3](=[O:30])[CH2:4][CH2:5][N:6]([C:23](OC(C)(C)C)=[O:24])[CH:7]1[CH2:12][CH2:11][N:10]([C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:14])[CH2:9][CH2:8]1>C(OCC)(=O)C>[O:24]=[C:23]1[NH:2][C:3](=[O:30])[CH2:4][CH2:5][N:6]1[CH:7]1[CH2:12][CH2:11][N:10]([C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:14])[CH2:9][CH2:8]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68425948Benzyl 4-[(3-amino-3-oxopropyl)(tert-butoxycarbonyl)amino]piperidin-1-carboxylate

생성물 1

HCID 68420297HCID 68420297, 화합물수율 98.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

4N Hydrogen chloride in ethyl acetate (4 mL) was added to a solution of benzyl 4-[(3-amino-3-oxopropyl)(tert-butoxycarbonyl)amino]piperidin-1-carboxylate (3.38 g) obtained in Example 45c) in ethyl acetate (16 mL), and the mixture was stirred at room temperature for 15 hours. The white solid (2.73 g) formed was collected by filtration. A solution of the resulting white solid (1.0 g), CDI (0.47 g) and DBU (0.89 g) in dichloroethane (30 mL) was refluxed for 15 hours. The reaction mixture was washed with an aqueous 5% citric acid solution and saturated saline solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to obtain the title compound (0.21 g, 21%) as a white powder.

출처 및 근거

ORD 기록
ord-9dd578aff7094bc785b5fdc099f805a3
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745623B2

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