1,1'-Thiocarbonyldiimidazole → 3-Isothiocyanato-4-methylthiophene

HRID 1825905ノート

反応式

HRID 1825905 の反応式
[NH2:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][CH:3]=1.C1N=CN([C:13](N2C=NC=C2)=[S:14])C=1>O1CCCC1>[CH3:7][C:6]1[C:2]([N:1]=[C:13]=[S:14])=[CH:3][S:4][CH:5]=1

参加物

4

反応物 2

HCID 802641,1'-ThiocarbonyldiimidazoleHCID 57433964-Methylthiophen-3-amine

生成物 1

HCID 221398273-Isothiocyanato-4-methylthiophene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-Methyl-3-thienyl isothiocyanate is obtained by reacting equimolar amounts of 3-amino-4-methylthiophene and N,N′-thiocarbonyldiimidazole in anhydrous tetrahydrofuran (THF) by stirring the reaction mixture at room temperature for 5 hours and then allowing the mixture to stand at room temperature overnight. 4-Methyl-3-thienyl isothiocyanate is isolated by distillative removal of the solvent under reduced pressure using a rotary evaporator, dissolving the residue in ethyl acetate and washing the organic phase repeatedly with water. The organic phase is dried over sodium sulfate and the organic solvent is then distilled off under reduced pressure using a rotary evaporator, giving 4-methyl-3-thienyl isothiocyanate as a brown oily residue. 4-Methyl-3-thienyl isothiocyanate can be used without further purification. b) N-(2-Amino-5-fluorophenyl)-N′-(4-methyl-3-thienyl)thiourea

後処理

  1. waitto stand at room temperature overnight

出典と根拠

ORDレコード
ord-3da4e0f2b7a84f2180fee1f21991edc2
出典データセット
uspto-grants-2006_05
特許番号
US07049333B2

反応ノート

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