Methyl isothiocyanate → HCID 178486101、化合物

HRID 66571ノート

反応式

HRID 66571 の反応式
[NH:1]([C:5]1[S:6][CH:7]=[C:8]([CH:10]2[CH2:15][CH2:14][CH2:13][CH:12]([NH2:16])[CH2:11]2)[N:9]=1)[C:2]([NH2:4])=[NH:3].[CH3:17][N:18]=[C:19]=[S:20].C(Cl)(Cl)Cl.CO.N>C(O)C>[NH:1]([C:5]1[S:6][CH:7]=[C:8]([CH:10]2[CH2:15][CH2:14][CH2:13][CH:12]([NH:16][C:19]([NH:18][CH3:17])=[S:20])[CH2:11]2)[N:9]=1)[C:2]([NH2:4])=[NH:3]

参加物

5

反応物 3

HCID 11167Methyl isothiocyanateHCID 21866414Chloroform methanol ammoniaHCID 1785126122-Guanidino-4-(3-aminocyclohexyl)thiazole

生成物 1

HCID 178486101HCID 178486101、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of 2-guanidino-4-(3-aminocyclohexyl)thiazole (0.6 g.) in ethanol (20 ml) was added methylisothiocyanate (0.18 g.) and the resulting solution was heated under reflux for two hours. The residue obtained on evaporation of the ethanol was subjected to column chromatography on silica gel (Kiesilgel 60, Merck) using chloroform/methanol/ammonia (s.g. 0.88) 8:2:0.3 v/v/v for development. The product, 2-guanidino-4-[3-(3-methylthioureido)cyclohexyl]thiazole, (0.4 g.) was obtained as a glass. The n.m.r. spectrum, in d6 dimethylsulphoxide, included resonances at 1.2-2.2(m,9H);2.8(d,3H); 4.0(m,1H); 6.2(s,1H); 6.8(br s,4H); and 7.2(br d,2H).

後処理

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux for two hours

出典と根拠

ORDレコード
ord-79818318c5b54ac58f64148de31b4973
出典データセット
uspto-grants-1982_08
特許番号
US04342765

反応ノート

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