3,4-Diaminopyridine → HCID 178503896、化合物

HRID 257423

反応式

HRID 257423 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[CH3:9][S:10][C:11](SC)=[N:12][C:13]#[N:14]>N1C=CC=CC=1>[CH3:9][S:10][C:11](=[N:12][C:13]#[N:14])[NH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8]

参加物

4

反応物 2

HCID 59183,4-DiaminopyridineHCID 66289Dimethyl N-cyanodithioiminocarbonate

生成物 1

HCID 178503896HCID 178503896、化合物収率 58%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3,4-Diaminopyridine (4 g, 36.6 mmol) was suspended in anhydrous pyridine (100 ml), and S,S'-dimethyl N-cyanodithioiminocarbonate (8.0 g, 55.0 mmol) was added thereto. The mixture was stirred at room temperature for 4 days. The resulting powder was collected from the reaction mixture by filtration, and washed with ether (100 ml) to obtain crude crystals. The crystals were purified by recrystallization from methanol-ether to obtain 1.91 g of the intended product as a white powder (yield: 58%). On the other hand, the filtrate was concentrated under reduced pressure, and the residue was purified by flash column chromatography (silica gel, eluent: chloroform:methanol=4:1 (v/v)) to obtain 2.8 g of the intended product (total yield: 95%).

後処理

  1. filtrationThe resulting powder was collected from the reaction mixture by filtration
  2. washwashed with ether (100 ml)
  3. customto obtain crude crystals
  4. customThe crystals were purified by recrystallization from methanol-ether

出典と根拠

ORDレコード
ord-9cb7892e7c7344dfae5c4dd0d1699a69
出典データセット
uspto-grants-1993_11
特許番号
US05262415

関連ノート

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