Hydrazine hydrate (1:1) → tert-Butyl 4-aminopiperazine-1-carboxylate

HRID 1904588노트

반응식

HRID 1904588 반응식
Cl[CH2:2][CH2:3][N:4]([CH2:12][CH2:13]Cl)[C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].O.[NH2:16][NH2:17].[Cl-].[NH4+]>>[NH2:16][N:17]1[CH2:13][CH2:12][N:4]([C:5]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:11])[CH2:3][CH2:2]1

참가 물질

4

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 25517Ammonium ChlorideHCID 11230235N-BOC-N,N-Bis(2-chloroethyl)amine

생성물 1

HCID 22029174tert-Butyl 4-aminopiperazine-1-carboxylate

실험 절차

Under an inert atmosphere at ambient temperature, 15.3 g of the product of Step A and 80 ml of hydrazine hydrate were mixed together and then 150 ml of a saturated aqueous solution of ammonium chloride were added. Extraction was done with methylene chloride and the organic phase was washed with an aqueous solution of ammonium chloride, dried, and the solvent was eliminated under reduced pressure. After chromatography on silica (eluent:methylene chloride - methanol, 100/7) 5 g of the expected product were obtained.

후처리

  1. extractionExtraction
  2. washthe organic phase was washed with an aqueous solution of ammonium chloride
  3. customdried

출처 및 근거

ORD 기록
ord-70d1a06436e74387b84703caec85fc7f
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839358

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