Acetic Acid → Acemetacin

HRID 1659165

反応式

HRID 1659165 の反応式
C(O[CH:5]([O:12][C:13](=[O:36])[CH2:14][C:15]1[C:23]2[C:18](=[CH:19][CH:20]=[C:21]([O:24][CH3:25])[CH:22]=2)[N:17]([C:26](=[O:34])[C:27]2[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=2)[C:16]=1[CH3:35])C1C=CC=CC=1)(=O)C.[C:37]([OH:40])(=[O:39])C>[C].[Pd]>[Cl:33][C:30]1[CH:31]=[CH:32][C:27]([C:26]([N:17]2[C:18]3[C:23](=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=3)[C:15]([CH2:14][C:13]([O:12][CH2:5][C:37]([OH:40])=[O:39])=[O:36])=[C:16]2[CH3:35])=[O:34])=[CH:28][CH:29]=1

参加物

4

反応物 2

HCID 176Acetic AcidHCID 70621351[1-(p-Chlorobenzoyl)-5-methoxy-2-methyl-3-indoleacetoxy]-benzyl acetate

生成物 1

HCID 1981Acemetacin

試薬・触媒・溶媒 1

HCID 178418390HCID 178418390、化合物触媒

実験手順

25.4 g (0.050 mol) of [1-(p-chlorobenzoyl)-5-methoxy-2-methyl-3-indoleacetoxy]-benzyl acetate were dissolved in 400 ml of glacial acetic acid and hydrogenated on 2.0 g of palladium carbon at room temperature. After the absorption of hydrogen had finished (1 hour), the catalyst was filtered off, the filtrate was concentrated by evaporation under vacuum and the compound was caused to crystallise by adding petroleum ether. The compound melted at 149.5°-150.5°C (determined on the micro-Kofler bench); the yield was 19.4 g which corresponds to 93% of the theoretical yield.

後処理

  1. customAfter the absorption of hydrogen
  2. custom(1 hour)
  3. filtrationthe catalyst was filtered off
  4. concentrationthe filtrate was concentrated by evaporation under vacuum
  5. customto crystallise
  6. additionby adding petroleum ether

出典と根拠

ORDレコード
ord-ab3ee72757984b029418cf8de4248ca2
出典データセット
uspto-grants-1976_06
特許番号
US03966956

関連ノート

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