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

HRID 1032012노트

반응식

HRID 1032012 반응식
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]

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-db653b2c27d94beb849404635ded44ba
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04956465

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