Diisopropylethylamine → N-(3-amino-4-thienyl)-N'-(4-methyl-3-thienyl)thiourea

HRID 349412ノート

反応式

HRID 349412 の反応式
Cl.Cl.[NH2:3][C:4]1[C:8]([NH2:9])=[CH:7][S:6][CH:5]=1.C(N(C(C)C)C(C)C)C.[CH3:19][C:20]1[C:21]([N:25]=[C:26]=[S:27])=[CH:22][S:23][CH:24]=1>O1CCCC1>[NH2:3][C:4]1[C:8]([NH:9][C:26]([NH:25][C:21]2[C:20]([CH3:19])=[CH:24][S:23][CH:22]=2)=[S:27])=[CH:7][S:6][CH:5]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 127073423,4-Diaminothiophene dihydrochlorideHCID 221398273-Isothiocyanato-4-methylthiophene

生成物 1

HCID 86037734N-(3-amino-4-thienyl)-N'-(4-methyl-3-thienyl)thiourea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 1.87 g of 3,4-diaminothiophene dihydrochloride, 60 ml of anhydrous tetrahydrofuran (THF) and 2.58 g of N-ethyl-N,N-diisopropylamine was stirred at room temperature for 30 minutes and then admixed with 1.5 g of 4-methyl-3-thienyl isothiocyanate. After stirring over approx. 18 hours, the solvent was distilled off, the residue admixed with water and extracted repeatedly with ethyl acetate. After the combined organic phases had been treated with activated carbon, they were dried over sodium sulfate and the solvent was once again distilled off. The N-(3-amino-4-thienyl)-N′-(4-methyl-3-thienyl)thiourea was obtained as an amorphous foamy solid.

後処理

  1. stirringAfter stirring over approx. 18 hours
  2. distillationthe solvent was distilled off
  3. extractionthe residue admixed with water and extracted repeatedly with ethyl acetate
  4. additionAfter the combined organic phases had been treated with activated carbon, they
  5. dry with materialwere dried over sodium sulfate
  6. distillationthe solvent was once again distilled off

出典と根拠

ORDレコード
ord-b42dad8b0c4d4bada62dd01825bed579
出典データセット
uspto-grants-2007_02
特許番号
US07179830B2

反応ノート

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