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

HRID 330980노트

반응식

HRID 330980 반응식
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

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0c86aa7825bf4cb9bc40e89065fb2c52
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877743B2

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