Potassium Carbonate → 2,2-Dimethylpropyl 4-{4-[amino(hydroxyimino)methyl]pyridin-2-yl}-1-piperazinecarboxylate

HRID 421821ノート

反応式

HRID 421821 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][N:6]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:16])[CH2:11][CH2:10]2)[CH:4]=1)#[N:2].Cl.[OH:24][NH2:25].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:2][C:1](=[N:25][OH:24])[C:3]1[CH:8]=[CH:7][N:6]=[C:5]([N:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:16])[CH2:13][CH2:14]2)[CH:4]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 119924192,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)-1-piperazinecarboxylate

生成物 1

HCID 1363817182,2-Dimethylpropyl 4-{4-[amino(hydroxyimino)methyl]pyridin-2-yl}-1-piperazinecarboxylate収率 110.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)piperazine-1-carboxylate (1.67 g) obtained in Example 2 was dissolved in ethanol (10 mL), and hydroxyamine hydrochloride (1.17 g) and potassium carbonate (3.11 g) were added thereto, heated under reflux for 2 hours, and the solvent was evaporated away, the resulting residue was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away to obtain 2.04 g of the entitled compound.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. customthe solvent was evaporated away
  4. additionthe resulting residue was diluted with ethyl acetate
  5. washwashed with water and saturated saline water
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe solvent was evaporated away

出典と根拠

ORDレコード
ord-7a9a6c8028c743b99639b3b27e6f6c45
出典データセット
uspto-grants-2012_01
特許番号
US08101618B2

反応ノート

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