Tetrabutylammonium Fluoride → 1-(4-Amino-2-chlorophenyl)ethanol

HRID 649840

반응식

HRID 649840 반응식
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.C[Si](C)(C)CCOC(=O)[NH:25][C:26]1[CH:31]=[CH:30][C:29]([CH:32]([OH:34])[CH3:33])=[C:28]([Cl:35])[CH:27]=1>O1CCCC1>[NH2:25][C:26]1[CH:31]=[CH:30][C:29]([CH:32]([OH:34])[CH3:33])=[C:28]([Cl:35])[CH:27]=1

참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 54096646[3-Chloro-4-(1-hydroxy-ethyl)-phenyl]carbamic acid 2-trimethylsilanyl-ethyl ester

생성물 1

HCID 185436011-(4-Amino-2-chlorophenyl)ethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 1M solution of tetrabutylammonium fluoride in tetrahydrofuran (5.7 mL) is added to [3-chloro-4(1-hydroxy-ethyl)-phenyl]-carbamic acid 2-trimethylsilanyl-ethyl ester (0.5 g) and the mixture is stirred at room temperature for approximately 3.5 hours. The solution is then concentrated under reduced pressure, dissolved in a 1:1 mixture of ethyl acetate and hexanes, washed successively with water then saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure followed by chromatography over silica gel (40% ethyl acetate in hexanes is used as the eluant) provides the product as an amber oil.

후처리

  1. concentrationThe solution is then concentrated under reduced pressure
  2. dissolutiondissolved in a 1:1 mixture of ethyl acetate and hexanes
  3. washwashed successively with water
  4. dry with materialsaturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate
  5. customRemoval of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-219944b111704ae2a454a9789c820987
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271236B1

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