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HCID 20532007、化合物 → HCID 20532008、化合物

HRID 1759368
ノート
印刷プレビュー

反応式

HRID 1759368 の反応式
[CH2:1]([C:4]1([C:13]([C:16]([O:18][C:19]2[CH:24]=[CH:23][C:22]([NH2:25])=[CH:21][CH:20]=2)=[O:17])([CH3:15])[CH3:14])[C:9](=[O:10])[NH:8][C:7](=[O:11])[NH:6][C:5]1=[O:12])[CH:2]=[CH2:3].[H][H]>[Pd].C(O)C>[CH2:1]([C:4]1([C:13]([C:16]([O:18][C:19]2[CH:20]=[CH:21][C:22]([NH2:25])=[CH:23][CH:24]=2)=[O:17])([CH3:15])[CH3:14])[C:9](=[O:10])[NH:8][C:7](=[O:11])[NH:6][C:5]1=[O:12])[CH2:2][CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 20532007HCID 20532007、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 20532008HCID 20532008、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of 750 g. of 5-allyl-5-(p-aminophenyloxycarbonyl-isopropyl)barbituric acid in 15 ml. of ethanol containing 100 mg. of 10% palladium-on-carbon as catalyst was subjected to hydrogenation at room temperature and atmospheric pressure. After one hour, the required amount (180 ml.) of hydrogen had been taken up. The reaction mixture was filtered through Celite, and the filtrate was evaporated to dryness. The residue was chromatographed on 13 g. of silica gel with ethyl acetate as the eluent. Fractions containing the desired product were evaporated. The remaining solid was recrystallized from chloroform/ether to afford 620 mg. (89%) of the ester, m.p. 212°-215°.

後処理

  1. customwas subjected to hydrogenation at room temperature
  2. filtrationThe reaction mixture was filtered through Celite
  3. customthe filtrate was evaporated to dryness
  4. customThe residue was chromatographed on 13 g
  5. additionFractions containing the desired product
  6. customwere evaporated
  7. customThe remaining solid was recrystallized from chloroform/ether
  8. customto afford 620 mg

出典と根拠

ORDレコード
ord-9eba8a93e59d45a581b72462ba8191fb
出典データセット
uspto-grants-1982_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04340736

反応ノート

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