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

HRID 1350755노트

반응식

HRID 1350755 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c0be285b2e644f6d8e94c21d0bfc47de
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214802B2

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