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

HRID 1825905

반응식

HRID 1825905 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 221398273-Isothiocyanato-4-methylthiophene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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

후처리

  1. waitto stand at room temperature overnight

출처 및 근거

ORD 기록
ord-3da4e0f2b7a84f2180fee1f21991edc2
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07049333B2

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