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

HRID 1904588ノート

反応式

HRID 1904588 の反応式
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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-70d1a06436e74387b84703caec85fc7f
出典データセット
uspto-grants-1989_06
特許番号
US04839358

反応ノート

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