tert-Butyl carbazate → Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate

HRID 2109260ノート

反応式

HRID 2109260 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.[C:9]([NH:16][NH2:17])([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10]>>[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[N:17][NH:16][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4][CH2:3]1

参加物

3

反応物 2

HCID 70091tert-Butyl carbazateHCID 740491-Methyl-4-piperidone

生成物 1

HCID 21097379Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate収率 32%

実験手順

A solution of 11.2 g (99.0 mmol) of 1-methyl-piperid-4-one and 13.0 g (100 mmol) of Boc-hydrazine in 150 mL of hexanes was refluxed for 30 minutes. The hot solution was dried over MgSO4, filtered, and allowed to cool. The resulting crystals were isolated and recrystallized from Et2O to provide 7.2 g of tert-butyl N′-(1-Methyl-piperidin-4-ylidene)-hydrazinecarboxylate as a white solid.

後処理

  1. dry with materialThe hot solution was dried over MgSO4
  2. filtrationfiltered
  3. temperatureto cool
  4. customThe resulting crystals were isolated
  5. customrecrystallized from Et2O

出典と根拠

ORDレコード
ord-bd36b320da88410b94f7e7655875b826
出典データセット
uspto-grants-2009_04
特許番号
US07514458B2

反応ノート

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