Water → HCID 13457754, 화합물

HRID 280126노트

반응식

HRID 280126 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 13457751HCID 13457751, 화합물

생성물 1

HCID 13457754HCID 13457754, 화합물수율 93.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

[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°.

후처리

  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

출처 및 근거

ORD 기록
ord-920887af67154f848a954690784215e8
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588727

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