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Diisopropylamine → (3S,4R)-1-(t-butyl dimethylsilyl)-3-(1-oxoethyl)-4-[2,2,2-tri(methylthio)ethyl]azetidin-2-one

HRID 64801
ノート
印刷プレビュー

反応式

HRID 64801 の反応式
C([Li])CCC.C(NC(C)C)(C)C.[Si:13]([N:20]1[C@@H:23]([CH2:24][C:25]([S:30][CH3:31])([S:28][CH3:29])[S:26][CH3:27])[CH2:22][C:21]1=[O:32])([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14].[C:33](N1C=CN=C1)(=[O:35])[CH3:34]>O1CCCC1>[Si:13]([N:20]1[C@H:23]([CH2:24][C:25]([S:28][CH3:29])([S:26][CH3:27])[S:30][CH3:31])[C@@H:22]([C:33](=[O:35])[CH3:34])[C:21]1=[O:32])([C:16]([CH3:17])([CH3:19])[CH3:18])([CH3:15])[CH3:14]
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

6

反応物 4

HCID 7912DiisopropylamineHCID 171741-(1H-Imidazol-1-yl)ethanoneHCID 13003465(4R)-1-(t-butyldimethylsilyl)-4-[2,2,2-tri(methylthio)ethyl]azetidin-2-oneHCID 178418339Butyllithium

生成物 1

HCID 14127274(3S,4R)-1-(t-butyl dimethylsilyl)-3-(1-oxoethyl)-4-[2,2,2-tri(methylthio)ethyl]azetidin-2-one

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
3 回

反応条件

温度
-78 °C

実験手順

n-Butyllithium (2.43 ml of 2.4 m solution, 5.84 mmol) is added by syringe to a solution of diisopropylamine (591 mg, 5.84 mmol) in 25 ml of freshly distilled tetrahydrofuran at -78° C. The resulting solution is stirred at -78° C. for 15 minutes prior to the addition of a solution of (4R)-1-(t-butyldimethylsilyl)-4-[2,2,2-tri(methylthio)ethyl]azetidin-2-one (1.00 g, 2.85 mmol) in tetrahydrofuran (5 ml). This solution is stirred at -78° C. for 15 minutes, then added via a Teflon tube to a mixture of N-acetylimidazole (642 mg, 5.84 mmol) in 25 ml of THF at -78° C. The resulting yellow reaction mixture is stirred at -78° C. for 10 minutes, then quenched by addition of saturated aqueous ammonium chloride solution. The mixture is diluted with ether (200 ml) and washed with 2.5N hydrochloric acid solution (50 ml), water (50 ml) and brine (50 ml) and dried over magnesium sulfate. Removal of solvents in vacuo gives a yellow oil which is chromatographed on silica gel (30% ether in petroleum ether) to yield (3S,4R)-1-(t-butyldimethylsilyl)-3-(1-oxoethyl)-4-[2,2,2-tri(methylthio)ethyl]azetidin-2-one. n.m.r. (CDCl3) δ4.42(m,1), δ4.32(d,1) δ2.35(m,2), δ2.32(s,3), δ2.2(s,9), δ0.98(s,9), δ0.3(2s,6).

後処理

  1. stirringThis solution is stirred at -78° C. for 15 minutes
  2. stirringThe resulting yellow reaction mixture is stirred at -78° C. for 10 minutes
  3. customquenched by addition of saturated aqueous ammonium chloride solution
  4. additionThe mixture is diluted with ether (200 ml)
  5. washwashed with 2.5N hydrochloric acid solution (50 ml), water (50 ml) and brine (50 ml)
  6. dry with materialdried over magnesium sulfate
  7. customRemoval of solvents in vacuo
  8. customgives a yellow oil which
  9. customis chromatographed on silica gel (30% ether in petroleum ether)

出典と根拠

ORDレコード
ord-94a57720b4ff46a2a200394f418b6a51
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04610820

反応ノート

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