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Cesium carbonate → Tert-butyl 4-(3-(diethoxyphosphoryl)propoxy)phenethylcarbamate

HRID 2407892
ノート
印刷プレビュー

反応式

HRID 2407892 の反応式
[OH:1][C:2]1[CH:17]=[CH:16][C:5]([CH2:6][CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:25][CH2:26][CH2:27][P:28](=[O:35])([O:32][CH2:33][CH3:34])[O:29][CH2:30][CH3:31]>CN(C=O)C>[CH2:33]([O:32][P:28]([CH2:27][CH2:26][CH2:25][O:1][C:2]1[CH:17]=[CH:16][C:5]([CH2:6][CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:12])[CH3:13])=[CH:4][CH:3]=1)([O:29][CH2:30][CH3:31])=[O:35])[CH3:34]
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 10796Cesium carbonateHCID 283500Diethyl (3-bromopropyl)phosphonateHCID 11831452tert-butyl N-(2-(4-hydroxyphenyl)ethyl)carbamate2 回

生成物 1

HCID 86678287Tert-butyl 4-(3-(diethoxyphosphoryl)propoxy)phenethylcarbamate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of tert-butyl 4-hydroxyphenethylcarbamate (1 eq) in DMF (0.17 M) was added cesium carbonate (5 eq). The resulting mixture was stirred at room temperature for 30 minutes, then diethyl 3-bromopropylphosphonate (1.2 eq) was added into the reaction mixture. The resulting mixture was stirred at room temperature for another 4 hours until tert-butyl 4-hydroxyphenethylcarbamate was consumed. The mixture was then diluted with ethyl acetate, and washed with 5% citric acid three times, saturated NaHCO3 solution, water and brine. The organic layer was then dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 80-100% EtOAc/Hex to give the product as a colorless oil.

後処理

  1. customwas consumed
  2. additionThe mixture was then diluted with ethyl acetate
  3. washwashed with 5% citric acid three times, saturated NaHCO3 solution, water and brine
  4. dry with materialThe organic layer was then dried over anhydrous Na2SO4
  5. concentrationconcentrated en vaccuo
  6. customThe crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO)

出典と根拠

ORDレコード
ord-ae4f523f3675481aaa274089a61af024
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08808703B2

反応ノート

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