ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methyl Acetate → (2S,4R)-N-tert-Butoxycarbonyl-4-tert-butyldimethylsiloxy-2-[1-hydroxy-2-(methoxycarbonyl)ethyl]pyrrolidine

HRID 1078722
ノート
印刷プレビュー

反応式

HRID 1078722 の反応式
C(N(CC)CCN(CC)CC)C.C[Si](C)(C)[N-][Si](C)(C)C.[Na+].[C:23]([O:26][CH3:27])(=[O:25])[CH3:24].[C:28]([O:32][C:33]([N:35]1[CH2:41][C@H:40]([O:42][Si:43]([C:46]([CH3:49])([CH3:48])[CH3:47])([CH3:45])[CH3:44])[CH2:39][C@H:36]1[CH:37]=[O:38])=[O:34])([CH3:31])([CH3:30])[CH3:29].[Cl-].[NH4+]>O1CCCC1>[C:28]([O:32][C:33]([N:35]1[CH2:41][C@H:40]([O:42][Si:43]([C:46]([CH3:49])([CH3:48])[CH3:47])([CH3:45])[CH3:44])[CH2:39][C@H:36]1[CH:37]([OH:38])[CH2:24][C:23]([O:26][CH3:27])=[O:25])=[O:34])([CH3:31])([CH3:30])[CH3:29]
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 5

HCID 6584Methyl AcetateHCID 25517Ammonium ChlorideHCID 674231,2-Ethanediamine, N1,N1,N2,N2-tetraethyl-HCID 2724254Sodium bis(trimethylsilyl)amideHCID 10969557tert-Butyl (2S,4R)-4-((tert-butyldimethylsilyl)oxy)-2-formylpyrrolidine-1-carboxylate

生成物 1

HCID 57107882
(2S,4R)-N-tert-Butoxycarbonyl-4-tert-butyldimethylsiloxy-2-[1-hydroxy-2-(methoxycarbonyl)ethyl]pyrrolidine
収率 87.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a mixture of tetrahydrofuran (45 ml) and tetraethylethylenediamine (1.5 ml) were successively added a 1.0M sodium hexamethyldisilazide--tetrahydrofuran solution (0.892 ml) and methyl acetate (71.2 μl) at -78° C. The mixture was stirred for 30 minutes, and then a tetrahydrofuran solution of (2S,4R)-N-tert-butoxycarbonyl-4-(tert-butyldimethylsiloxy)prolinal (196 mg) was added thereto. This solution was stirred for 30 minutes. Saturated aqueous ammonium chloride was added to the reaction solution. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (heptane-ethyl acetate=3:1) to obtain the title compound [209 mg, yield: 87.1%; (R)-isomer (polar compound):(S)-isomer (less polar compound)=1.82:1].

後処理

  1. customat -78° C
  2. stirringThis solution was stirred for 30 minutes
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was removed in vacuo
  7. customThe residue was purified by silica gel column chromatography (heptane-ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-1da1f5a7568c451280c191a38c8cb6a9
出典データセット
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05550121

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート