Ammonium Chloride → HCID 9816246, 화합물

HRID 1934351노트

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HRID 1934351 반응식
[CH:1]([C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:5])[CH3:4])=[O:2].[CH3:17][Mg]Br.[Cl-].[NH4+]>C1COCC1>[OH:2][CH:1]([CH3:17])[C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:5])[CH3:4]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 9794544HCID 9794544, 화합물HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 9816246HCID 9816246, 화합물수율 86%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of N-(1-formyl-1-methylethyl)-2,4-difluorobenzamide obtained in Example 32 (1.14 g, 5 mmol) in THF (10 ml) was added 0.9 M methyl magnesium bromide in THF (13 ml, 12 mmol) dropwise at −20° C. The reaction mixture was warmed gradually to room temperature over 2 hours and added to 10% aqueous ammonium chloride (100 ml). The resulting mixture was extracted with ethyl acetate, washed with saturated aqueous NaHCO3 and brine, dried over MgSO4, concentrated under a reduced pressure and the residue was crystallized from hexane/ethyl acetate to give the title compound (1.05 g; 86%).

후처리

  1. extractionThe resulting mixture was extracted with ethyl acetate
  2. washwashed with saturated aqueous NaHCO3 and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under a reduced pressure
  5. customthe residue was crystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-a6b2ecf4a0b54ea897b9aefd8cc9c65f
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06384033B1

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