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Dimethylformamide → N-tert-butoxycarbonyl 1-(2-formyl-5-fluorobenzofur-7-yl)-2-aminopropane

HRID 1824952
ノート
印刷プレビュー

反応式

HRID 1824952 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH3:21])[CH2:10][C:11]1[C:19]2[O:18][CH:17]=[CH:16][C:15]=2[CH:14]=[C:13]([F:20])[CH:12]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([Li])CCC.CN(C)[CH:29]=[O:30]>O1CCCC1>[C:1]([O:5][C:6]([NH:8][CH:9]([CH3:21])[CH2:10][C:11]1[C:19]2[O:18][C:17]([CH:29]=[O:30])=[CH:16][C:15]=2[CH:14]=[C:13]([F:20])[CH:12]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 22144858N-tert-butoxycarbonyl 1-(5-fluorobenzofur-7-yl)-2-aminopropaneHCID 178418339Butyllithium

生成物 1

HCID 22144756N-tert-butoxycarbonyl 1-(2-formyl-5-fluorobenzofur-7-yl)-2-aminopropane収率 69.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 0.50 gm (1.7 mMol) N-tert-butoxycarbonyl 1-(5-fluorobenzofur-7-yl)-2-aminopropane in 75 mL tetrahydrofuran was cooled to −78° C. under a nitrogen atmosphere. To this solution were then added 2.4 mL (3.81 mMoL) n-butyllithium (1.6 M in hexane) dropwise, resulting in an orange solution. After 5 minutes 0.66 mL (8.52 mMol) dimethylformamide were added dropwise. After stirring 18 hours at room temperature the reaction mixture was quenched by addition of 20 mL saturated aqueous ammonium chloride. The reaction mixture was partitioned between 300 mL ethyl acetate and 300 mL water. The phases were separated and the aqueous phase was extracted twice with 200 mL ethyl acetate. The organic phases were combined and washed sequentially with two 200 mL portions of water and one 200 mL portion of saturated aqueous sodium chloride, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with hexane containing 20% ethyl acetate. Fractions containing product were combined and concentrated under reduced pressure to provide 0.38 gm (69%) of the desired compound as a yellow solid.

後処理

  1. customresulting in an orange solution
  2. customwas quenched by addition of 20 mL saturated aqueous ammonium chloride
  3. customThe reaction mixture was partitioned between 300 mL ethyl acetate and 300 mL water
  4. customThe phases were separated
  5. extractionthe aqueous phase was extracted twice with 200 mL ethyl acetate
  6. washwashed sequentially with two 200 mL portions of water and one 200 mL portion of saturated aqueous sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. washeluting with hexane containing 20% ethyl acetate
  10. additionFractions containing product
  11. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-84214047547a47e78455cd7cfb5e1762
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07045545B1

反応ノート

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