Potassium Carbonate → [3-(4-Chloro-phenyl)-allyl]-(3,4-difluoro-benzyl)-amine

HRID 597878노트

반응식

HRID 597878 반응식
C(OC(=O)[N:7]([CH2:17][CH:18]=[CH:19][C:20]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=1)[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([F:15])=[C:11]([F:16])[CH:10]=1)(C)(C)C.C([O-])([O-])=O.[K+].[K+]>Cl.O1CCOCC1>[Cl:26][C:23]1[CH:22]=[CH:21][C:20]([CH:19]=[CH:18][CH2:17][NH:7][CH2:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([F:16])[CH:10]=2)=[CH:25][CH:24]=1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 67271108[3-(4-Chloro-phenyl)-allyl]-(3,4-difluoro-benzyl)-carbamic acid tert-butyl ester

생성물 1

HCID 67271292[3-(4-Chloro-phenyl)-allyl]-(3,4-difluoro-benzyl)-amine수율 97.9%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

A solution of [3-(4-chloro-phenyl)-allyl]-(3,4-difluoro-benzyl)-carbamic acid tert-butyl ester (2.04 g) in 20 mL of 4N HCl in dioxane was stirred at room temperature for 1 hr. The solution was poured into 150 mL of aq. K2CO3, and extracted with 3×50 mL of ethyl acetate. The combined organic layer was washed with 50 mL brine, dried over Na2SO4, filtered and concentrated to provide 1.49 g of [3-(4-chloro-phenyl)-allyl]-(3,4-difluoro-benzyl)-amine.

후처리

  1. extractionextracted with 3×50 mL of ethyl acetate
  2. washThe combined organic layer was washed with 50 mL brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-78dae3b997d646d796b8ecd46b25316a
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897601B2

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