Water → HCID 13457754、化合物

HRID 280126ノート

反応式

HRID 280126 の反応式
[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[C:4]([C:6]1[N:7]([N:11](C)[C:12](=O)OCC)[CH:8]=[CH:9][CH:10]=1)=[O:5].O.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[C:4]([C:6]1[N:7]([NH:11][CH3:12])[CH:8]=[CH:9][CH:10]=1)=[O:5]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 13457751HCID 13457751、化合物

生成物 1

HCID 13457754HCID 13457754、化合物収率 93.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

[2-(2-Chlorobenzoyl)-1H-pyrrol-1-yl]-methyl-carbamic acid, ethyl ester (39.2 g, 0.127 mol) was dissolved in 100 ml of ethanol and 200 ml of H2O containing sodium hydroxide (25 g, 0.625 mol). The reaction was refluxed for 18 hours followed by evaporation of the ethanol. The aqueous solution was extracted with three 300 ml portions of ethyl acetate, dried (MgSO4), filtered, and evaporated to give 28 g of an oil. This oil was distilled via Kugelrohr apparatus 125° (0.15 mmHg) to give 26.3 g of a solid. This solid was triturated with hexane to give 25.5 g (85%) of crystals, m.p. 56°-58°.

後処理

  1. temperatureThe reaction was refluxed for 18 hours
  2. customfollowed by evaporation of the ethanol
  3. extractionThe aqueous solution was extracted with three 300 ml portions of ethyl acetate
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-920887af67154f848a954690784215e8
出典データセット
uspto-grants-1986_05
特許番号
US04588727

反応ノート

読み込み中…