Hydrazine hydrate (1:1) → 1-Piperidinecarboxylic acid, 4-[2-(aminooxy)ethoxy]-, 1,1-dimethylethyl ester

HRID 1053356ノート

反応式

HRID 1053356 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH2:13][CH2:14][O:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:18][CH2:17]1.O.NN>C(O)C.C(Cl)Cl>[NH2:3][O:12][CH2:13][CH2:14][O:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:18][CH2:17]1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86693960tert-Butyl 4-{2-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]ethoxy}piperidine-1-carboxylate

生成物 1

HCID 866939611-Piperidinecarboxylic acid, 4-[2-(aminooxy)ethoxy]-, 1,1-dimethylethyl ester収率 86%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 4-{2-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]ethoxy}piperidine-1-carboxylate 70 (0.57 g, 1.46 mmol) in a mixture of ethanol (1 mL) and DCM (6 mL) was added hydrazine hydrate (0.086 g, 1.46 mmol). The reaction mixture was stirred at room temperature for 16 h. Precipitate was filtered off. The filtrate was evaporated and the residue was subjected to chromatography to give 71 (0.327 g, 86%) as a colorless oil.

後処理

  1. filtrationPrecipitate was filtered off
  2. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-17bdf86ac44c44cfaab73fd37df6b2f2
出典データセット
uspto-grants-2016_07
特許番号
US09393239B2

反応ノート

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