N-Methoxy-N-methyl-5-phenylethynylnicotinamide → HCID 67047758, 화합물

HRID 606867노트

반응식

HRID 606867 반응식
[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

참가 물질

5

반응물 2

HCID 86076555N-Methoxy-N-methyl-5-phenylethynylnicotinamideHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 67047758HCID 67047758, 화합물수율 84%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 25517Ammonium Chloride용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-61449d423ab94c7cbd02057cad914deb
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915424B2

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