Hydrochloric Acid → HCID 178444387、化合物

HRID 621396

反応式

HRID 621396 の反応式
Cl.[CH2:2]([C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([NH2:15])=[NH:14])[CH2:9][CH2:8]1)[CH2:3][CH2:4][CH2:5][CH3:6].[CH3:16][O:17][CH:18]([C:23](OC)=[O:24])[C:19](OC)=[O:20].C[O-].[Na+].Cl>CO>[CH2:2]([C@H:7]1[CH2:8][CH2:9][C@H:10]([C:13]2[N:15]=[C:23]([OH:24])[C:18]([O:17][CH3:16])=[C:19]([OH:20])[N:14]=2)[CH2:11][CH2:12]1)[CH2:3][CH2:4][CH2:5][CH3:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 78718Dimethyl methoxymalonateHCID 10942334Sodium MethoxideHCID 178444523HCID 178444523、化合物

生成物 1

HCID 178444387HCID 178444387、化合物収率 76.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

This trans-4-pentylcyclohexanecarboxamidine hydrochloride (69 g, 0.30 mol) and dimethyl methoxymalonate (48 g, 0.30 mol) were added to a solution of sodium methylate (56 g, 1.0 mol) dissolved in anhydrous methanol (1 l), followed by heating the mixture under reflux with stirring for 5 hours, thereafter cooling the resulting material, mixing it with 6N-hydrochloric acid (500 ml), agitating the mixed liquid at room temperature for 20 minutes, filtering the liquid under suction through a filter, washing the resulting residue on the filter with water and methanol and drying it under reduced pressure to obtain 2-(trans-4-pentylcyclohexyl)-4,6-dihydroxy-5-methoxypyrimidine (67 g, 0.23 mol).

後処理

  1. temperatureby heating the mixture
  2. temperatureunder reflux
  3. temperaturecooling the resulting material
  4. stirringagitating the mixed liquid at room temperature for 20 minutes
  5. filtrationfiltering the liquid under suction through a filter
  6. washwashing the resulting residue on the
  7. filtrationfilter with water and methanol
  8. customdrying it under reduced pressure

出典と根拠

ORDレコード
ord-75d317e262074094992716415ffca4bd
出典データセット
uspto-grants-1989_04
特許番号
US04824596

関連ノート

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