Dichloromethane → Di-tert-butyl 4-(aminooxy)pyrazolidine-1,2-dicarboxylate

HRID 330980ノート

反応式

HRID 330980 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH:13]1[CH2:17][N:16]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[N:15]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:14]1.C(Cl)Cl.O.NN>C(O)C>[NH2:3][O:12][CH:13]1[CH2:14][N:15]([C:25]([O:27][C:28]([CH3:29])([CH3:30])[CH3:31])=[O:26])[N:16]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 86694006di-tert-butyl 4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]pyrazolidine-1,2-dicarboxylate

生成物 1

HCID 86694007Di-tert-butyl 4-(aminooxy)pyrazolidine-1,2-dicarboxylate収率 83%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of di-tert-butyl 4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]pyrazolidine-1,2-dicarboxylate 142 (1.81 g, 4.18 mmol) in a solution of DCM (20 mL) and ethanol (4 mL) was added hydrazine hydrate (0.240 mL, 4.18 mmol) at room temperature. The mixture was stirred at room temperature overnight, filtered and concentrated to provide a residue which was subjected to chromatography to give 143 (1.04 g, 83%) as a white foam.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated
  3. customto provide a residue which

出典と根拠

ORDレコード
ord-0c86aa7825bf4cb9bc40e89065fb2c52
出典データセット
uspto-grants-2014_11
特許番号
US08877743B2

反応ノート

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