Lawesson's reagent → HCID 57973784、化合物

HRID 1863929ノート

反応式

HRID 1863929 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][C:11](=O)[C:6]2=[N:5][N:4]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>>[F:1][C:2]([F:14])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][C:11](=[S:24])[C:6]2=[N:5][N:4]=1

参加物

3

反応物 2

HCID 87949Lawesson's reagentHCID 685205773-(trifluoromethyl)-6,7-dihydro-[1,2,4]triazolo[4,3-a]pyrazin-8(5H)-one

生成物 1

HCID 57973784HCID 57973784、化合物

実験手順

A mixture of 173 mg (0.84 mmol) of 3-(trifluoromethyl)-6,7-dihydro[1,2,4]triazolo[4,3-a]pyrazin-8(5H)-one, 703 mg (1.68 mmol) of Lawesson's Reagent, and 18 mL of xylenes was stirred at reflux for 4.5 h. After being cooled to room temperature, the solvent was decanted off, and the residue was washed with diethyl ether. The resulting solid was dried and purified by flash chromatography (20-50% acetone in hexanes) to give the title compound as a greenish-yellow solid. LC-MS 223 (M+1).

後処理

  1. temperatureat reflux for 4.5 h
  2. customthe solvent was decanted off
  3. washthe residue was washed with diethyl ether
  4. customThe resulting solid was dried
  5. custompurified by flash chromatography (20-50% acetone in hexanes)

出典と根拠

ORDレコード
ord-2b6cf08764ab4a38a980079c14365388
出典データセット
uspto-grants-2009_12
特許番号
US07625888B2

反応ノート

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