Hydrazine hydrate (1:1) → 5-Amino-2-(3-aminopropyl)-3-methylpyridine

HRID 1607045

반응식

HRID 1607045 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH3:14])[C:7]([CH2:10][CH2:11][C:12]#[N:13])=[N:8][CH:9]=1)([O-])=O.O.NN>[Ni].C(O)C>[NH2:1][C:4]1[CH:5]=[C:6]([CH3:14])[C:7]([CH2:10][CH2:11][CH2:12][NH2:13])=[N:8][CH:9]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)2회HCID 198517775-Nitro-2-(2-cyanoethyl)-3-methylpyridine

생성물 1

HCID 198517805-Amino-2-(3-aminopropyl)-3-methylpyridine수율 145.2%

시약·촉매·용매 2

HCID 935Nickel촉매2회HCID 702Ethanol용매2회

실험 절차

Raney nickel (24 g) was added to a stirred solution under nitrogen of 5-nitro-2-(2-cyanoethyl)-3-methylpyridine (10.36 g) in ethanol (700 ml). Hydrazine hydrate (13.5 ml) in ethanol (30 ml) was added over 2.75 hr., followed by further additions of Raney nickel (15 g) and hydrazine hydrate (60 ml) over two days which included two periods of eight hours at 50° C. The solution was decanted off, filtered through a hyflo pad and concentrated to dryness to give a green oil (13 g). This oil was chromatographed on silica in ethylacetate/ethanol/0.880 ammonia 15:10:2 to give the title compound as an oil (8.14 g).

후처리

  1. customtwo periods of eight hours
  2. customat 50° C
  3. customThe solution was decanted off
  4. filtrationfiltered through a hyflo pad
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-f6fda4fb51ba4b879b6e5c579f866115
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863933

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