Lawesson's reagent → (E)-4-Methyl-1-[4-[7-(trifluoromethyl)-4-quinolyl]piperazin-1-yl]hex-2-ene-1-thione

HRID 333986노트

반응식

HRID 333986 반응식
[CH3:1][CH:2]([CH2:27][CH3:28])/[CH:3]=[CH:4]/[C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[C:22]3[C:17](=[CH:18][C:19]([C:23]([F:26])([F:25])[F:24])=[CH:20][CH:21]=3)[N:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:38])=CC=1>C1COCC1>[CH3:1][CH:2]([CH2:27][CH3:28])/[CH:3]=[CH:4]/[C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[C:22]3[C:17](=[CH:18][C:19]([C:23]([F:26])([F:25])[F:24])=[CH:20][CH:21]=3)[N:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)=[S:38]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 86691602(E)-4-Methyl-1-[4-[7-(trifluoromethyl)-4-quinolyl]piperazin-1-yl]hex-2-en-1-one

생성물 1

HCID 86691603(E)-4-Methyl-1-[4-[7-(trifluoromethyl)-4-quinolyl]piperazin-1-yl]hex-2-ene-1-thione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

(E)-4-methyl-1-[4-[7-(trifluoromethyl)-4-quinolyl]piperazin-1-yl]hex-2-en-1-one (20 mg, 0.049 mmol) was dissolved in THF (1 ml), Lawesson's reagent (20 mg, 0.051 mmol) was added in one portion and the resulting mixture was stirred overnight at room temperature. The volatiles were removed under reduced pressure and the residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 5.4 mg (0.013 mmol, 25%).

후처리

  1. customThe volatiles were removed under reduced pressure
  2. customthe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
  3. customto yield 5.4 mg (0.013 mmol, 25%)

출처 및 근거

ORD 기록
ord-a87e0d5970434aa18618f7618bdc92fd
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883791B2

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