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

HRID 330930ノート

反応式

HRID 330930 の反応式
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

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-533611b5d2c74655a501eea0280e7aff
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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