Hydrochloric Acid → HCID 22248020, 화합물

HRID 890039

반응식

HRID 890039 반응식
C1(OP([CH:17](NC2C=CC=CC=2)[C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)(=O)OC2C=CC=CC=2)C=CC=CC=1.[F:31][C:32]1[C:33]([CH:37]=O)=[CH:34][S:35][CH:36]=1.C(=O)([O-])[O-:40].[Cs+].[Cs+].Cl.[OH-].[Na+]>O1CCCC1CCCO>[F:31][C:32]1[C:33]([CH2:37][C:17]([C:18]2[CH:19]=[CH:20][N:21]=[CH:22][CH:23]=2)=[O:40])=[CH:34][S:35][CH:36]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 14798Sodium HydroxideHCID 423769Diphenyl (phenylamino)(pyridin-4-yl)methylphosphonateHCID 22247846614729-75-8

생성물 1

HCID 22248020HCID 22248020, 화합물수율 36%

시약·촉매·용매 1

HCID 130202-Furanpropanol, tetrahydro-용매

실험 절차

After dissolving 19.6 g of [(phenylamino)-(4-pyridylmethyl)]phosphonic acid diphenyl ester [CAS No.3360-72-3] in 115 ml of tetrahydrofuran-2-propanol (4:1), 6.02 g of 4-fluorothiophene-3-carboxaldehyde and 19.61 g of anhydrous cesium carbonate were added and the mixture was stirred overnight at room temperature. Next, 90 ml of 5N hydrochloric acid was added to the reaction mixture and the mixture was stirred at room temperature for 6 hours. After adding a 5N sodium hydroxide solution to the reaction solution, extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate). The obtained solid was washed with n-hexane to obtain the title compound (3.66 g, 36% yield).

후처리

  1. stirringthe mixture was stirred at room temperature for 6 hours
  2. extractionto the reaction solution, extraction
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate)
  7. washThe obtained solid was washed with n-hexane

출처 및 근거

ORD 기록
ord-62ad8f8894364847877351c556aca5cb
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995144B2

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