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Ammonium Chloride → HCID 15735660、化合物

HRID 704611
ノート
印刷プレビュー

反応式

HRID 704611 の反応式
[CH:1]1(/[CH:7]=[C:8](\[CH2:12][P:13]([OH:19])([CH2:15][CH:16]([CH3:18])[CH3:17])=[O:14])/[C:9]([OH:11])=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1CCN2C(=NCCC2)CC1.[C:31]([O:37][CH2:38]Cl)(=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33].[Cl-].[NH4+]>CN(C)C=O.ClCCl.CO.C(O)(=O)C>[CH:1]1(/[CH:7]=[C:8](\[CH2:12][P:13]([OH:19])([CH2:15][CH:16]([CH3:17])[CH3:18])=[O:14])/[C:9]([O:11][CH2:38][O:37][C:31](=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33])=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 87885Chloromethyl pivalateHCID 15735587HCID 15735587、化合物

生成物 1

HCID 15735660HCID 15735660、化合物収率 64.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide
溶媒
HCID 21877243DCM MeOH AcOH溶媒

実験手順

To a solution of 100 mg (0.347 millimole) of (Z)-3-cyclohexyl-2-(hydroxyisobutylphosphinoyl)methylpropenoic acid in 1.0 ml of dimethylformamide were added 130 μl (0.87 millimole) of 1,8-diazabicyclo[5,4,0]-7-undecene and 75 μl (0.52 millimole) of chloromethyl pivalate, and the mixture was stirred at room temperature for 21 hours. Fifty milliliters of a saturated aqueous solution of ammonium chloride was added to the reaction mixture, and the mixture was extracted three times with 30 ml of ethyl acetate each time. The combined organic layers were washed with 10 ml of a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by preparative thin-layer chromatography silica gel 60 F254 made by E. Merck & Co.; dichloromethane/methanol/acetic acid [30:1:1)] to give 90 mg (yield 64%) of the captioned compound as a colorless oil.

後処理

  1. extractionthe mixture was extracted three times with 30 ml of ethyl acetate each time
  2. washThe combined organic layers were washed with 10 ml of a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by preparative thin-layer chromatography silica gel 60 F254

出典と根拠

ORDレコード
ord-8556b961c32b43c797607a00d6d7b13e
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04988681

反応ノート

読み込み中…

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