Hydrochloric Acid → HCID 68420297、化合物

HRID 20243ノート

反応式

HRID 20243 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 68420297HCID 68420297、化合物収率 98.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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.

出典と根拠

ORDレコード
ord-9dd578aff7094bc785b5fdc099f805a3
出典データセット
uspto-grants-2010_06
特許番号
US07745623B2

反応ノート

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