Triphenylphosphine → 6-(3,5-difluorophenyl)-2-[3-(5-methylpyridin-2-yl)benzyl]-2H-pyridazin-3-one

HRID 1408389

反応式

HRID 1408389 の反応式
N(C(OC(C)C)=O)=NC(OC(C)C)=O.[CH3:15][C:16]1[CH:17]=[CH:18][C:19]([C:22]2[CH:23]=[C:24]([CH2:28]O)[CH:25]=[CH:26][CH:27]=2)=[N:20][CH:21]=1.[F:30][C:31]1[CH:32]=[C:33]([C:38]2[CH:39]=[CH:40][C:41](=[O:44])[NH:42][N:43]=2)[CH:34]=[C:35]([F:37])[CH:36]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[F:30][C:31]1[CH:32]=[C:33]([C:38]2[CH:39]=[CH:40][C:41](=[O:44])[N:42]([CH2:28][C:24]3[CH:25]=[CH:26][CH:27]=[C:22]([C:19]4[CH:18]=[CH:17][C:16]([CH3:15])=[CH:21][N:20]=4)[CH:23]=3)[N:43]=2)[CH:34]=[C:35]([F:37])[CH:36]=1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 25241749HCID 25241749、化合物HCID 56604357(3-(5-Methylpyridin-2-yl)phenyl)methanol

生成物 1

HCID 594848946-(3,5-difluorophenyl)-2-[3-(5-methylpyridin-2-yl)benzyl]-2H-pyridazin-3-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.2 134 mg (0.66 mmol) of diisopropyl azodicarboxylate are added to a solution of 88 mg (0.44 mmol) of [3-(5-methylpyridin-2-yl)phenyl]methanol, 138 mg (0.66 mmol) of 6-(3,5-difluorophenyl)-2H-pyridazin-3-one and 174 mg (0.66 mmol) of triphenylphosphine in 3.5 ml of THF. The reaction mixture is stirred at room temperature for 18 hours. The mixture is evaporated, and the residue is chromatographed on a silica gel column with dichloromethane/methanol as eluent: 6-(3,5-difluorophenyl)-2-[3-(5-methylpyridin-2-yl)benzyl]-2H-pyridazin-3-one (“A9”) as colourless crystals; ESI 390.

後処理

  1. customThe mixture is evaporated
  2. customthe residue is chromatographed on a silica gel column with dichloromethane/methanol as eluent

出典と根拠

ORDレコード
ord-d9f3a906aada457db5444dbcb73fdcff
出典データセット
uspto-grants-2014_12
特許番号
US08921357B2

関連ノート

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