Lawesson's reagent → HCID 57973784, 화합물

HRID 1863929노트

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HRID 1863929 반응식
[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

참가 물질

3

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-2b6cf08764ab4a38a980079c14365388
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625888B2

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