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

HRID 333986ノート

反応式

HRID 333986 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-a87e0d5970434aa18618f7618bdc92fd
出典データセット
uspto-grants-2014_11
特許番号
US08883791B2

反応ノート

読み込み中…