Hydrochloric Acid → HCID 57656563, 화합물

HRID 911594노트

반응식

HRID 911594 반응식
Cl.O1CCOCC1.C(OC([NH:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23](=[O:29])[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[CH:19][C:18]=1[F:30])=O)(C)(C)C.C([O-])(O)=O.[Na+]>ClCCl>[CH3:26][C:25]([CH3:28])([CH3:27])[CH2:24][C:23]([C:20]1[CH:21]=[CH:22][C:17]([CH2:16][NH2:15])=[C:18]([F:30])[CH:19]=1)=[O:29]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 57656601HCID 57656601, 화합물

생성물 1

HCID 57656563HCID 57656563, 화합물수율 101.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Add 4N hydrogen chloride in dioxane (5.5 mL, 22 mmol) to a solution of N-(tert-butoxycarbonyl)-4-(3,3-dimethyl-butyryl)-2-fluoro-benzylamine (600 mg, 1.85 mmol) in dichloromethane (22 mL) and stir for 6.5 h. Concentrate in vacuo and wash the solid obtained with diethyl ether. Suspend the solid into saturated aqueous NaHCO3 and stir for 30 min. Extract the aqueous phase twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to obtain the title compound as an oil (420 mg, 99%).

후처리

  1. concentrationConcentrate in vacuo
  2. washwash the solid
  3. customobtained with diethyl ether
  4. stirringstir for 30 min
  5. extractionExtract the aqueous phase twice with EtOAc
  6. dry with materialDry the combined organic extracts over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-1d008622a3b1413d9eea17401871c20d
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022062B2

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