Hydrochloric Acid → 4-Hydrazinyl-1-methylpiperidine

HRID 2109261

반응식

HRID 2109261 반응식
B.[CH3:2][N:3]1[CH2:8][CH2:7][C:6](=[N:9][NH:10]C(OC(C)(C)C)=O)[CH2:5][CH2:4]1.Cl>C1COCC1>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([NH:9][NH2:10])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6331BoraneHCID 21097379Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate

생성물 1

HCID 109205354-Hydrazinyl-1-methylpiperidine수율 81.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

A solution of 1 M borane in THF (30 mL) was added to solid 2.80 g (12.3 mmol) of tert-butyl N′-(1-Methyl-piperidin-4-ylidene)-hydrazinecarboxylate. The mixture was stirred under N2 for 16 h when 40 mL of 6M HCl was carefully added. The mixture was heated to 60° C. for 30 min. The mixture was concentrated in vacuo at ambient temperature for 2 days. Petroleum ether (200 mL) and powdered NaOH (5 g) were added, and the mixture was stirred manually for 30 min. The mixture was dried with MgSO4, filtered, and carefully concentrated to give 1.3 g of (1-methyl-piperidin-4-yl)-hydrazine.

후처리

  1. additionwas carefully added
  2. concentrationThe mixture was concentrated in vacuo at ambient temperature for 2 days
  3. additionPetroleum ether (200 mL) and powdered NaOH (5 g) were added
  4. dry with materialThe mixture was dried with MgSO4
  5. filtrationfiltered
  6. concentrationcarefully concentrated

출처 및 근거

ORD 기록
ord-7b6ff192016d496fbf220b53c76b1f33
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07514458B2

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