Hydrochloric Acid → Ethyl 8-cyano-7-(cyano-ethoxycarbonyl-methyl-)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinoline-carboxylate

HRID 1032012ノート

反応式

HRID 1032012 の反応式
Cl[C:2]1[C:11]([C:12]#[N:13])=[C:10]2[C:5]([C:6](=[O:22])[C:7]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:8][N:9]2[CH:14]2[CH2:16][CH2:15]2)=[CH:4][C:3]=1[F:23].[C:24]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])#[N:25].CC(C)([O-])C.[K+].Cl>O1CCOCC1>[C:12]([C:11]1[C:2]([CH:26]([C:24]#[N:25])[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:3]([F:23])[CH:4]=[C:5]2[C:10]=1[N:9]([CH:14]1[CH2:16][CH2:15]1)[CH:8]=[C:7]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]2=[O:22])#[N:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7764Ethyl cyanoacetateHCID 23431783Ethyl 7-chloro-8-cyano-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 14422907Ethyl 8-cyano-7-(cyano-ethoxycarbonyl-methyl-)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinoline-carboxylate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2.8 g of ethyl 7-chloro-8-cyano-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinoline-carboxylate and 1.92 g of ethyl cyanoacetate are initially introduced into 30 ml of dioxane. 1.91 g of potassium tert-butoxide are metered in at room temperature. The mixture is stirred overnight and then ice-water is added. It is rendered acidic using HCl and extracted using methylene chloride. The organic phase is dried and concentrated. The residue is stirred once more with water and the solid is isolated.

後処理

  1. customare metered in at room temperature
  2. extractionextracted
  3. customThe organic phase is dried
  4. concentrationconcentrated
  5. stirringThe residue is stirred once more with water
  6. customthe solid is isolated

出典と根拠

ORDレコード
ord-db653b2c27d94beb849404635ded44ba
出典データセット
uspto-grants-1990_09
特許番号
US04956465

反応ノート

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