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Trimethylsilyl isocyanate → N-tert-butoxycarbonyl 1-(2-trimethylsilyl-5-fluorobenzofur-7-yl)-2-aminopropane

HRID 1824953
ノート
印刷プレビュー

反応式

HRID 1824953 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.[CH3:27][Si:28](N=C=O)([CH3:30])[CH3:29]>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]([Si:28]([CH3:30])([CH3:29])[CH3:27])=[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 70696Trimethylsilyl isocyanateHCID 22144858N-tert-butoxycarbonyl 1-(5-fluorobenzofur-7-yl)-2-aminopropaneHCID 178418339Butyllithium

生成物 1

HCID 22144822N-tert-butoxycarbonyl 1-(2-trimethylsilyl-5-fluorobenzofur-7-yl)-2-aminopropane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 0.20 gm (0.68 mMol) N-tert-butoxycarbonyl 1-(5-fluorobenzofur-7-yl)-2-aminopropane in 10 mL tetrahydrofuran was cooled to −78° C. under a nitrogen atmosphere. To this solution were then added 0.96 mL (1.53 mMoL) n-butyllithium (1.6 M in hexane) dropwise, resulting in an orange solution. After 50 minutes 0.14 mL (1.02 mMol) trimethylsilylisocyanate were added dropwise. After 15 minutes the reaction mixture was quenched by addition of 2 mL saturated aqueous ammonium chloride and was then allowed to warm to room temperature. The reaction mixture was partitioned between 150 mL ethyl acetate and 150 mL water. The phases were separated and the organic phase was washed sequentially with 150 mL water and 150 mL saturated aqueous sodium chloride, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with 10:1 hexane:ethyl acetate. Fractions containing product were combined and concentrated under reduced pressure to provide the desired compound.

後処理

  1. customresulting in an orange solution
  2. customAfter 15 minutes the reaction mixture was quenched by addition of 2 mL saturated aqueous ammonium chloride
  3. customThe reaction mixture was partitioned between 150 mL ethyl acetate and 150 mL water
  4. customThe phases were separated
  5. washthe organic phase was washed sequentially with 150 mL water and 150 mL saturated aqueous sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. washeluting with 10:1 hexane
  9. additionFractions containing product
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-bc894d499de04055bb386ca0200bbf07
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

読み込み中…

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