Water → 2-(2,2,2-Trifluoroethoxy)ethyl p-toluenesulfonate

HRID 1175258ノート

反応式

HRID 1175258 の反応式
[F:1][C:2]([F:9])([F:8])[CH2:3][O:4][CH2:5][CH2:6][OH:7].[S:10](Cl)([C:13]1[CH:19]=[CH:18][C:16]([CH3:17])=[CH:15][CH:14]=1)(=[O:12])=[O:11].O>N1C=CC=CC=1>[CH3:17][C:16]1[CH:18]=[CH:19][C:13]([S:10]([O:7][CH2:6][CH2:5][O:4][CH2:3][C:2]([F:9])([F:8])[F:1])(=[O:12])=[O:11])=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 2558542-(2,2,2-Trifluoroethoxy)ethan-1-ol

生成物 1

HCID 220332952-(2,2,2-Trifluoroethoxy)ethyl p-toluenesulfonate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2-(2,2,2-trifluoroethoxy)ethanol (intermediate BR) (12.7 g) was dissolved in anhydrous pyridine, then TsCl (1.3 eq) was added, and the mixture was stirred at room temperature for 16 h, after which TLC showed the reaction was complete. Then the mixture was poured into water, extracted with EA, washed with water and brine, and dried with anhydrous Na2SO4. The solvent was removed and the residue purified by column chromatography to obtain intermediate BS (0.3 g).

後処理

  1. extractionextracted with EA
  2. washwashed with water and brine
  3. dry with materialdried with anhydrous Na2SO4
  4. customThe solvent was removed
  5. customthe residue purified by column chromatography
  6. customto obtain intermediate BS (0.3 g)

出典と根拠

ORDレコード
ord-c550af2456a74ca7a98e0a65b713054b
出典データセット
uspto-grants-2010_11
特許番号
US07838499B2

反応ノート

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