N-Methoxy-N-methyl-5-phenylethynylnicotinamide → HCID 67047758、化合物

HRID 606867ノート

反応式

HRID 606867 の反応式
[CH3:1][Mg]Br.CON(C)[C:7](=[O:22])[C:8]1[CH:13]=[C:12]([C:14]#[C:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:11]=[N:10][CH:9]=1>C(OCC)(=O)C.[Cl-].[NH4+]>[C:16]1([C:15]#[C:14][C:12]2[CH:13]=[C:8]([C:7](=[O:22])[CH3:1])[CH:9]=[N:10][CH:11]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 2

HCID 86076555N-Methoxy-N-methyl-5-phenylethynylnicotinamideHCID 178418573HCID 178418573、化合物

生成物 1

HCID 67047758HCID 67047758、化合物収率 84%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 25517Ammonium Chloride溶媒

実験手順

Add methylmagnesium bromide (1.25 mL, 3.7 mmol) dropwise at 0° C. to a solution of N-methoxy-N-methyl-5-phenylethynylnicotinamide, (prepared essentially as described in PREPARATION 2), (1.0 g, 3.76 mmol). Allow the mixture to warn to room temperature overnight. Dilute with ethyl acetate and saturated ammonium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 10:90 to 30:70 tetrahydrofuran:hexanes) to give title compound as a white solid (0.70 g, 84%).

後処理

  1. custom(prepared essentially
  2. customas described in PREPARATION 2), (1.0 g, 3.76 mmol)
  3. dry with materialdry (magnesium sulfate)
  4. concentrationconcentrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with 10:90 to 30:70 tetrahydrofuran:hexanes)

出典と根拠

ORDレコード
ord-61449d423ab94c7cbd02057cad914deb
出典データセット
uspto-grants-2011_03
特許番号
US07915424B2

反応ノート

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