Acetic Acid → HCID 19895670, 화합물

HRID 1073875노트

반응식

HRID 1073875 반응식
[CH3:1][C:2]1([CH3:19])[CH:7]=[C:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[O:3]1.C(O)(=O)C>C(O)C.[Pd]>[CH3:1][C:2]1([CH3:19])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[O:3]1

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 19895692HCID 19895692, 화합물

생성물 1

HCID 19895670HCID 19895670, 화합물수율 46.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

2.97 g of 2,2-dimethyl-4-(3-methyl-2-pyridyl)-2H-1benzopyran were dissolved in 50 ml of ethanol and shaken at room temperature under a hydrogen atmosphere with 10% palladium-on-charcoal in the presence of 0.5 ml of acetic acid. After 24 hours the catalyst was filtered off and the filtrate was evaporated. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. There were obtained 1.4 g of 3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl) -2H-1-benzopyran together with mixed fractions containing this compound and starting material. The procedure described above was carried out on the mixed fractions to give 675 mg of 3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl) -2H-1-benzopyran which was recrystallized from t-butyl methyl ether and then melted at 100-102° C.

후처리

  1. filtrationAfter 24 hours the catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was chromatographed on silica gel
  4. washfor the elution

출처 및 근거

ORD 기록
ord-64e28b4229114ddebdd6ee909e5e30ce
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971982

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