3,4-Diaminopyridine → HCID 178503896, 화합물

HRID 257423

반응식

HRID 257423 반응식
[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]

참가 물질

4

반응물 2

HCID 59183,4-DiaminopyridineHCID 66289Dimethyl N-cyanodithioiminocarbonate

생성물 1

HCID 178503896HCID 178503896, 화합물수율 58%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9cb7892e7c7344dfae5c4dd0d1699a69
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262415

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