Borane → (1-Tert-butyl-piperidin-4-yl)-hydrazine

HRID 2109272노트

반응식

HRID 2109272 반응식
B.C1COCC1.C(OC([NH:14][N:15]=[C:16]1[CH2:21][CH2:20][N:19]([C:22]([CH3:25])([CH3:24])[CH3:23])[CH2:18][CH2:17]1)=O)(C)(C)C>Cl>[C:22]([N:19]1[CH2:18][CH2:17][CH:16]([NH:15][NH2:14])[CH2:21][CH2:20]1)([CH3:25])([CH3:23])[CH3:24]

참가 물질

5

반응물 3

HCID 6331BoraneHCID 8028TetrahydrofuranHCID 48916874Tert-butyl 2-(1-tert-butylpiperidin-4-ylidene)hydrazinecarboxylate

생성물 1

HCID 21097250(1-Tert-butyl-piperidin-4-yl)-hydrazine

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
60 °C

실험 절차

A 1M solution borane in THF (28.7 mL, 28.7 mmol) was added to N′-(1-tert-Butyl-piperidin-4-ylidene)-hydrazinecarboxylic acid tert-butyl ester. The mixture was stirred for 16 h, and then 40 mL of 6M HCl was added. The mixture was heated to 60° C. for 30 min. The mixture was concentrated and 200 mL of petroleum ether was added, followed by powdered NaOH (5 g). The slurry was stirred manually for 30 min, and then the mixture was dried with MgSO4, filtered, and concentrated to give 1.21 g of (1-tert-butyl-piperidin-4-yl)-hydrazine (1.21 g).

후처리

  1. concentrationThe mixture was concentrated
  2. addition200 mL of petroleum ether was added
  3. stirringThe slurry was stirred manually for 30 min
  4. dry with materialthe mixture was dried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b9e6f9eca0e3440ab86fb9bf9bcafa43
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07514458B2

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