Dichloromethane → Di-tert-butyl{[4-(aminooxy)piperidin-1-yl]methylylidene}biscarbamate

HRID 1053352노트

반응식

HRID 1053352 반응식
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([NH:28][C:29](=[O:35])[O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[N:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:15][CH2:14]1.C(Cl)Cl.O.NN>C(O)C>[NH2:3][O:12][CH:13]1[CH2:14][CH2:15][N:16]([C:19]([NH:28][C:29](=[O:35])[O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[N:20][C:21](=[O:27])[O:22][C:23]([CH3:25])([CH3:26])[CH3:24])[CH2:17][CH2:18]1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 86699594Di-tert-butyl [{4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]piperidin-1-yl}methylylidene]biscarbamate

생성물 1

HCID 86699595Di-tert-butyl{[4-(aminooxy)piperidin-1-yl]methylylidene}biscarbamate수율 43%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture di-tert-butyl [{4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]piperidin-1-yl}methylylidene]biscarbamate 64 (2.30 g, 4.71 mmol) in a solution of DCM (40 mL) and ethanol (6 mL) was added hydrazine hydrate (0.270 mL, 4.71 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 65 (0.72 g, 43%) as a white foam.

후처리

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

출처 및 근거

ORD 기록
ord-053ccdb0a02e4875b107b9fc513e668b
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09393239B2

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