Formic Acid → 3-(5-bromo-thiophen-2-yl)-1-methyl-1H-[1,2,4]triazole

HRID 1020954ノート

反応式

HRID 1020954 の反応式
[CH3:1][NH:2][NH:3][C:4]([C:6]1[S:7][C:8]([Br:11])=[CH:9][CH:10]=1)=[NH:5].[CH:12](O)=O>>[Br:11][C:8]1[S:7][C:6]([C:4]2[N:5]=[CH:1][N:2]([CH3:12])[N:3]=2)=[CH:10][CH:9]=1

参加物

3

反応物 2

HCID 284Formic AcidHCID 178486232HCID 178486232、化合物

生成物 1

HCID 583719633-(5-bromo-thiophen-2-yl)-1-methyl-1H-[1,2,4]triazole

実験手順

A mixture of compound 5-bromo-thiophene 2-carboximidic-N′-methyl-hydrazide (4BW) (13 g) in formic acid (100 ml) was refluxed overnight and concentrated. The residue was treated with sat. NaHCO3, and extracted with EtOAc three times. The combined organics were dried over MgSO4. After concentration, compound 5BW was purified by column using 80% EtoAc/hexane to yield light yellow colored solid.

後処理

  1. temperaturewas refluxed overnight
  2. concentrationconcentrated
  3. additionThe residue was treated with sat. NaHCO3
  4. extractionextracted with EtOAc three times
  5. dry with materialThe combined organics were dried over MgSO4
  6. concentrationAfter concentration, compound
  7. customwas purified by column
  8. customto yield light yellow colored solid

出典と根拠

ORDレコード
ord-88744a2cbbf34795ae70be31c1465d12
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

反応ノート

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