Sodium Methoxide → HCID 21182511, 화합물

HRID 1386617노트

반응식

HRID 1386617 반응식
CN([CH:4]=[CH:5][C:6](=O)[C:7]1[CH:12]=[CH:11][C:10]([C:13]([O:15][CH2:16]C)=[O:14])=[CH:9][CH:8]=1)C.Cl.[CH2:20]([O:26][C:27]1[CH:35]=[CH:34][C:30]([C:31]([NH2:33])=[NH:32])=[CH:29][CH:28]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C[O-].[Na+]>CO>[CH2:20]([O:26][C:27]1[CH:28]=[CH:29][C:30]([C:31]2[N:33]=[CH:4][CH:5]=[C:6]([C:7]3[CH:12]=[CH:11][C:10]([C:13]([O:15][CH3:16])=[O:14])=[CH:9][CH:8]=3)[N:32]=2)=[CH:34][CH:35]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

참가 물질

5

반응물 3

HCID 10942334Sodium MethoxideHCID 12238501p-n-Hexyloxybenzamidine hydrochlorideHCID 54211795HCID 54211795, 화합물

생성물 1

HCID 21182511HCID 21182511, 화합물수율 52.1%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a suspension of 1-(N,N-dimethylamino)-2-(4-ethoxycarbonylbenzoyl)ethylene (0.742 g) and 4-n-hexyloxybenzamidine hydrochloride (0.847 g) in methanol (10 ml) was added 28% sodium methoxide in methanol (0.64 ml). The suspension was refluxed for 6 hours, and partitioned with ethyl acetate and water. The organic layer was washed with water and brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with acetonitrile, collected by filtration and dried under reduced pressure to give Methyl 4-[2-(4-n-hexyloxyphenyl)pyrimidin-6-yl]benzoate (0.61 g).

후처리

  1. temperatureThe suspension was refluxed for 6 hours
  2. custompartitioned with ethyl acetate and water
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was triturated with acetonitrile
  7. filtrationcollected by filtration
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-6059b437672d4236be52109495d66445
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265536B1

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