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Toluene → Tert-butyl 3-cyclohexylmethyl-4-(4-isopropyl-2-oxooxazolidin-3-yl)-4-oxobutyrate

HRID 1060743
ノート
印刷プレビュー

反応式

HRID 1060743 の反応式
C[Si](C)(C)[N-][Si](C)(C)C.[Na+].C1(C)C=CC=CC=1.[CH:18]1([CH2:24][CH2:25][C:26]([N:28]2[C@@H:32]([CH:33]([CH3:35])[CH3:34])[CH2:31][O:30][C:29]2=[O:36])=[O:27])[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.[C:37]([O:41][C:42](=[O:45])[CH2:43]Br)([CH3:40])([CH3:39])[CH3:38]>C1COCC1.Cl>[CH:18]1([CH2:24][CH:25]([C:26]([N:28]2[CH:32]([CH:33]([CH3:34])[CH3:35])[CH2:31][O:30][C:29]2=[O:36])=[O:27])[CH2:43][C:42]([O:41][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:45])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]1
参加物反応条件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 1140TolueneHCID 79177tert-Butyl bromoacetateHCID 2724254Sodium bis(trimethylsilyl)amideHCID 69156991(S)-3-cyclohexylpropionyl-4-isopropyloxazolidin-2-one

生成物 1

HCID 18628724Tert-butyl 3-cyclohexylmethyl-4-(4-isopropyl-2-oxooxazolidin-3-yl)-4-oxobutyrate収率 61%

試薬・触媒・溶媒 2

HCID 313
Hydrochloric Acid
溶媒
HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-10 °C

実験手順

A solution of sodium hexamethyldisilazide (92.4 mL of a 0.6M toluene solution, Aldrich) in THF (70 mL) was cooled to −78° C. and then treated with a solution of (S)-3-cyclohexylpropionyl-4-isopropyloxazolidin-2-one (10.5 g, 39.3 mmol) in THF (30 mL) added dropwise over 10 minutes. The mixture was stirred for 1 hour and then treated with a solution of tert-butylbromoacetate (9.75 mL, 50 mmol) in THF (20 mL) added dropwise. The mixture was stirred for 1 hour, while warming to −10° C. The mixture reaction was diluted with 1M hydrochloric acid (100 mL) and the dilution was extracted with ethyl acetate (200 mL). The extract was washed with saturated aqueous sodium bicarbonate (100 mL) and brine (100 mL), dried (MgSO4), filtered and concentrated to dryness. The residue was dissolved in hexane and product was crystallized out to provide tert-butyl 3-cyclohexylmethyl-4-(4-isopropyl-2-oxooxazolidin-3-yl)-4-oxobutyrate (9.09 g, 61%). MS (M+1): 382.

後処理

  1. additionadded dropwise over 10 minutes
  2. additionadded dropwise
  3. stirringThe mixture was stirred for 1 hour
  4. customThe mixture reaction
  5. extractionthe dilution was extracted with ethyl acetate (200 mL)
  6. washThe extract was washed with saturated aqueous sodium bicarbonate (100 mL) and brine (100 mL)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated to dryness
  10. dissolutionThe residue was dissolved in hexane
  11. customproduct was crystallized out

出典と根拠

ORDレコード
ord-09da4d66629e49eabacfb64ab6fe6c0a
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06525036B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート