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

HRID 597878ノート

反応式

HRID 597878 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-78dae3b997d646d796b8ecd46b25316a
出典データセット
uspto-grants-2011_03
特許番号
US07897601B2

反応ノート

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