Iodine → HCID 178485021、化合物

HRID 1758804ノート

反応式

HRID 1758804 の反応式
[OH-].[Na+].Cl.[CH3:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[CH2:10][SH:11].[C:12]([NH:14][C:15]([NH:20][CH3:21])=[N:16][CH2:17][CH2:18][SH:19])#[N:13].II>>[C:12]([NH:14][C:15]([NH:20][CH3:21])=[N:16][CH2:17][CH2:18][S:19][S:11][CH2:10][C:6]1[N:7]=[CH:8][NH:9][C:5]=1[CH3:4])#[N:13]

参加物

5

反応物 4

HCID 807Iodine2 回HCID 14798Sodium HydroxideHCID 159163955-Methyl-4-mercaptomethylimidazole hydrochlorideHCID 178485018HCID 178485018、化合物

生成物 1

HCID 178485021HCID 178485021、化合物

実験手順

Aqueous sodium hydroxide (3.60 g, 0.9 mol) was added to a stirred ethanolic solution of 5-methyl-4-mercaptomethylimidazole hydrochloride (5.92 g, 0.03 mol) and N-cyano-N'-methyl-N"-(2-mercaptoethyl)guanidine (5.74 g, 0.0363 mol). The solution was cooled to 0° and a saturated ethanolic solution of iodine was added until the iodine color remained. The solvent was removed under reduced pressure to yield an oil which was purified using preparative high pressure liquid chromatography (silica gel; 13% methanol in ethyl acetate). The glassy product obtained was triturated with acetonitrile to yield N-cyano-N'-methyl-N"-[2-(5-methyl-4-imidazolylmethyldithio)ethyl]guanidine, m.p. 137°-142°; Ms m/e 284.

後処理

  1. temperatureThe solution was cooled to 0°
  2. customThe solvent was removed under reduced pressure
  3. customto yield an oil which
  4. customwas purified
  5. customThe glassy product obtained
  6. customwas triturated with acetonitrile

出典と根拠

ORDレコード
ord-6a79da242988423995e5bcfe2deb664b
出典データセット
uspto-grants-1983_02
特許番号
US04374996

反応ノート

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