Ethanol → HCID 13457765、化合物

HRID 280137ノート

反応式

HRID 280137 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]([CH3:17])C(=O)OCC)[CH:8]=[CH:9][CH:10]=1)=[O:5].[OH-].[Na+].[CH2:24](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][CH3:17])[C:8]([CH3:24])=[CH:9][CH:10]=1)=[O:5]

参加物

4

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 13457751HCID 13457751、化合物

生成物 1

HCID 13457765HCID 13457765、化合物

実験手順

A solution containing [2-(2-chlorobenzoyl)-1H-pyrrol-1-yl]-methyl-carbamic acid, ethyl ester (29.4 g, 91 mmol) and sodium hydroxide (11 g, 275 mmol) in 50% aqueous ethanol was heated under reflux for 16 hours. The excess ethanol was evaporated and the solution was adjusted to pH 7 with 10% HCl. The resultant slurry was extracted with three 100 ml portions of DCM, dried (MgSO4), filtered, and evaporated to give 22 g of solid. This solid was charcoaled and recrystallized from ether-hexane to give 21 g (93%) of powder, m.p. 107°-108°.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. customThe excess ethanol was evaporated
  4. extractionThe resultant slurry was extracted with three 100 ml portions of DCM
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-b335e86a9f724589b90de3b9624cf7ba
出典データセット
uspto-grants-1986_05
特許番号
US04588727

反応ノート

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