Propargylamine → HCID 178457409、化合物

HRID 27380

反応式

HRID 27380 の反応式
[N+:1]([CH:4]=[C:5](SC)[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2].[CH2:19]([NH2:22])[C:20]#[CH:21]>C(#N)C>[N+:1]([CH:4]=[C:5]([NH:22][CH2:19][C:20]#[CH:21])[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 239041PropargylamineHCID 178503826HCID 178503826、化合物

生成物 1

HCID 178457409HCID 178457409、化合物収率 87%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene prepared according to Belgian Pat. No. 814,941 (4.0 g, 0.014 mole) and distilled propargylamine (7.74 g, 0.14 mole) in acetonitrile (60 ml) was stirred at reflux temperature under a positive pressure of nitrogen for 18 hours. The reaction mixture was cooled, evaporated to dryness and then triturated under 20 ml of isopropyl alcohol to give the title compound (3.58 g, 87%). Column chromatography on silica gel by gradient elution using methylene chloride-methanol gave a pure sample; mp 159°-160° dec.

後処理

  1. customprepared
  2. temperatureat reflux temperature under a positive pressure of nitrogen for 18 hours
  3. temperatureThe reaction mixture was cooled
  4. customevaporated to dryness
  5. customtriturated under 20 ml of isopropyl alcohol

出典と根拠

ORDレコード
ord-988f2b78e6134f9c8ad9f36d5d102635
出典データセット
uspto-grants-1980_09
特許番号
US04221737

関連ノート

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