Diethyl (ethoxymethylene)malonate → HCID 178450108、化合物

HRID 1195613ノート

反応式

HRID 1195613 の反応式
Cl.[CH2:2]([O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=[NH:12])=[CH:9][CH:8]=1)[CH2:3][CH2:4][CH3:5].C([O:18][CH:19]=[C:20]([C:26](OCC)=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22])C.C[O-].[Na+].CO.[Na]>CO>[CH2:24]([O:23][C:21]([C:20]1[C:19]([OH:18])=[N:12][C:11]([C:10]2[CH:14]=[CH:15][C:7]([O:6][CH2:2][CH2:3][CH2:4][CH3:5])=[CH:8][CH:9]=2)=[N:13][CH:26]=1)=[O:22])[CH3:25]

参加物

6

反応物 4

HCID 6871Diethyl (ethoxymethylene)malonateHCID 3015453Benzamidine, p-butoxy-, monohydrochloride2 回HCID 5360545SodiumHCID 23694274Sodium methanolate methanol

生成物 1

HCID 178450108HCID 178450108、化合物収率 69.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

4-Butyloxybenzamidine hydrochloride (II) (22.9 g, 0.1 mol) and diethyl ethoxymethylenemalonate (III) (23.8 g, 0.1 mol) were suspended in methanol (100 ml), followed by agitating the suspension while keeping it at 10° C., dropwise adding a sodium methoxide-methanol solution, separately prepared by reacting sodium (2.5 g, 0.11 mol) with methanol (200 ml), then agitating the mixture for 2.5 hours, distilling off methanol under reduced pressure, gradually adding 6N-hydrochloric acid till the solution reached a pH of 4, filtering the resulting white precipitate, washing the precipitate with a small quantity of methanol and drying the precipitate to obtain ethyl-2-(4-butyloxyphenyl)-4-hydroxy-5-pyrimidinecarboxylate (IV) (21.9 g) (yield: 69% based on compound (II)).

後処理

  1. customat 10° C.
  2. customseparately prepared
  3. stirringagitating the mixture for 2.5 hours
  4. distillationdistilling off methanol under reduced pressure
  5. additiongradually adding 6N-hydrochloric acid till the solution
  6. filtrationfiltering the resulting white precipitate
  7. washwashing the precipitate with a small quantity of methanol
  8. customdrying the precipitate

出典と根拠

ORDレコード
ord-b4776067836c483d8a8a14b6c5de21f1
出典データセット
uspto-grants-1992_05
特許番号
US05112523

反応ノート

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