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

Water → (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-methoxymethylpyrrolidine

HRID 1029636
ノート
印刷プレビュー

反応式

HRID 1029636 の反応式
[H-].[Na+].[CH3:3]I.[Si:5]([O:12][C@H:13]1[CH2:17][N:16]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C@H:15]([CH2:25][OH:26])[CH2:14]1)([C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:7])[CH3:6].O>O1CCCC1.C(OCC)(=O)C>[Si:5]([O:12][C@H:13]1[CH2:17][N:16]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C@H:15]([CH2:25][O:26][CH3:3])[CH2:14]1)([C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:7])[CH3:6]
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 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 11078078tert-butyl (2S,4R)-4-((tert-butyldimethylsilyl)oxy)-2-(hydroxymethyl)pyrrolidine-1-carboxylate

生成物 1

HCID 15117246(2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-methoxymethylpyrrolidine

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of sodium hydride (60% in oil, 816 mg) and methyl iodide (4.9 ml) in tetrahydrofuran (50 ml), which was heated at 50°-60° C., was added dropwise a solution of (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-hydroxymethylpyrrolidine (5.2 g) in tetrahydrofuran (10 ml). After stirring for two hours, the reaction mixture was poured into a mixture of water and ethyl acetate, the organic layer was separated, washed in turn with saturated aqueous sodium sulfite and brine, dried over magnesium sulfate. Evaporation of the solvent gave an oil, which was chromatographed on silica gel (200 ml) eluting with a mixture of hexane and ethyl acetate (4:1, V/V) to give (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-methoxymethylpyrrolidine (4.5 g).

後処理

  1. customthe organic layer was separated
  2. washwashed in turn with saturated aqueous sodium sulfite and brine
  3. dry with materialdried over magnesium sulfate
  4. customEvaporation of the solvent
  5. customgave an oil, which
  6. customwas chromatographed on silica gel (200 ml)
  7. washeluting with a mixture of hexane and ethyl acetate (4:1, V/V)

出典と根拠

ORDレコード
ord-6e76b26e11be456abe287a565d7403c6
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05102877

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