Sodium Methoxide → HCID 21182511、化合物

HRID 1386617ノート

反応式

HRID 1386617 の反応式
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]

参加物

5

反応物 3

HCID 10942334Sodium MethoxideHCID 12238501p-n-Hexyloxybenzamidine hydrochlorideHCID 54211795HCID 54211795、化合物

生成物 1

HCID 21182511HCID 21182511、化合物収率 52.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6059b437672d4236be52109495d66445
出典データセット
uspto-grants-2001_07
特許番号
US06265536B1

反応ノート

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