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

HRID 2250481

反応式

HRID 2250481 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

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.

後処理

  1. customis obtained
  2. waitto stand at room temperature overnight

出典と根拠

ORDレコード
ord-3a08955c9ba74d3c9c1e5bc9c5618295
出典データセット
uspto-grants-2008_01
特許番号
US07317033B2

関連ノート

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