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

HRID 34927

反応式

HRID 34927 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 198517805-Amino-2-(3-aminopropyl)-3-methylpyridine収率 145.2%

試薬・触媒・溶媒 2

HCID 935Nickel触媒2 回HCID 702Ethanol溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e65b65387f754e1a8c83ddf37853aff1
出典データセット
uspto-grants-1988_08
特許番号
US04764519

関連ノート

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