Water → HCID 58293359、化合物

HRID 1912407ノート

反応式

HRID 1912407 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH:10]([C:13]([OH:15])=[O:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[C:23]([F:27])([F:26])[CH:24]=[CH2:25].O>CN(C)C=O>[F:26][C:23]([F:27])=[CH:24][CH2:25][O:14][C:13]([CH:10]1[CH2:11][CH2:12][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[CH2:9]1)=[O:15]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 5550853-bromo-3,3-difluoroprop-1-eneHCID 27605291-((Tert-butoxy)carbonyl)pyrrolidine-3-carboxylic acid

生成物 1

HCID 58293359HCID 58293359、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To a solution of pyrrolidine-1,3-dicarboxylic acid-1-tert-butyl ester (3.40 g) in N,N-dimethylformamide (34 ml) were added potassium carbonate (4.37 g) and 3-bromo-3,3-difluoropropene (1.93 ml), and the mixture was stirred at 60° C. for 6 hours. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=5/1) to give the titled compound (3.73 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=5/1)

出典と根拠

ORDレコード
ord-9634fa3c2ab3488ca8e059c2d36329d5
出典データセット
uspto-grants-2013_12
特許番号
US08609647B2

反応ノート

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