Sodium → HCID 178433684、化合物

HRID 426680ノート

反応式

HRID 426680 の反応式
[Na].C([NH:4][C:5]([NH:10]C)=[N:6][CH2:7][CH2:8][SH:9])#N.Cl.[CH3:13][C:14]1[NH:18][CH:17]=[N:16][C:15]=1[CH2:19]Cl>C(O)C>[CH3:13][C:14]1[NH:18][CH:17]=[N:16][C:15]=1[CH2:19][S:9][CH2:8][CH2:7][NH:6][C:5]([NH2:10])=[NH:4]

参加物

5

反応物 3

HCID 5360545Sodium2 回HCID 124562084-(Chloromethyl)-5-methyl-1H-imidazole--hydrogen chloride (1/1)HCID 178485018HCID 178485018、化合物

生成物 1

HCID 178433684HCID 178433684、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Sodium (1.43 g) was added, with stirring under nitrogen, to dry ethanol (100 ml). After the sodium had dissolved a solution of N-cyano-N'-methyl-N"-(2-mercaptoethyl)guanidine (4.90 g) in dry ethanol (50 ml) was added and the mixture was stirred at room temperature for one hour. 5-Methyl-4-chloromethylimidazole hydrochloride (5.18 g) was added in batches over a period of one hour at room temperature. The mixture was then stirred at room temperature, for a further hour and heated at reflux temperature for 1/2 hour. After cooling the mixture was filtered and the filtrate was evaporated to a glassy solid (8.8 g). This crude product was chromatographed on silica gel with acetonitrile as eluant and the solid product obtained (3.60 g) was recrystallised from acetonitrile to give N-cyano-N'-methyl-"-[2-(5-methyl-4-imidazolylmethylthio)ethyl]guanidine, m.p.=140°-142° C.

後処理

  1. additionwas added
  2. stirringThe mixture was then stirred at room temperature, for a further hour
  3. temperatureheated
  4. temperatureat reflux temperature for 1/2 hour
  5. temperatureAfter cooling the mixture
  6. filtrationwas filtered
  7. customthe filtrate was evaporated to a glassy solid (8.8 g)
  8. customThis crude product was chromatographed on silica gel with acetonitrile as eluant
  9. customthe solid product obtained (3.60 g)
  10. customwas recrystallised from acetonitrile

出典と根拠

ORDレコード
ord-289fae7ef0c64c3c90b42c42d6198b75
出典データセット
uspto-grants-1979_10
特許番号
US04171325

反応ノート

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