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

HRID 2400637ノート

反応式

HRID 2400637 の反応式
[C:1]([O:5][C:6](=[O:35])[NH:7][C:8]([N:17]1[CH2:22][CH2:21][CH:20]([O:23][N:24]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:19][CH2:18]1)=[N:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:4])([CH3:3])[CH3:2].C(Cl)Cl.O.NN>C(O)C>[C:12]([O:11][C:10](=[O:16])[NH:9][C:8]([N:17]1[CH2:18][CH2:19][CH:20]([O:23][NH2:24])[CH2:21][CH2:22]1)=[N:7][C:6](=[O:35])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:13])([CH3:14])[CH3:15]

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-cb0432e0401e4166a93620eb3221575c
出典データセット
uspto-grants-2014_08
特許番号
US08796257B2

反応ノート

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