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N-Methylacetamide → HCID 22865001、化合物

HRID 1078727
ノート
印刷プレビュー

反応式

HRID 1078727 の反応式
[CH3:1][NH:2][C:3](=[O:5])[CH3:4].CN(C)P(=O)(N(C)C)N(C)C.C([N-]C(C)C)(C)C.[Li+].[C:25]([O:29][C:30]([N:32]1[CH2:38][C@H:37]([O:39][Si:40]([C:43]([CH3:46])([CH3:45])[CH3:44])([CH3:42])[CH3:41])[CH2:36][C@H:33]1[CH:34]=[O:35])=[O:31])([CH3:28])([CH3:27])[CH3:26]>O1CCCC1.C(OCC)(=O)C.O.O>[C:25]([O:29][C:30]([N:32]1[CH2:38][C@H:37]([O:39][Si:40]([C:43]([CH3:46])([CH3:45])[CH3:44])([CH3:42])[CH3:41])[CH2:36][C@H:33]1[CH:34]([OH:35])[CH2:4][C:3](=[O:5])[NH:2][CH3:1])=[O:31])([CH3:28])([CH3:27])[CH3:26]
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

8

反応物 4

HCID 6582N-MethylacetamideHCID 12679HexamethylphosphoramideHCID 2724682Lithium diisopropylamideHCID 10969557tert-Butyl (2S,4R)-4-((tert-butyldimethylsilyl)oxy)-2-formylpyrrolidine-1-carboxylate

生成物 1

HCID 22865001HCID 22865001、化合物収率 25.9%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒4 回
HCID 22728543Water ethylacetate溶媒

反応条件

温度
-78 °C

実験手順

Under a nitrogen atmosphere, a solution of N-methylacetamide (116 μl, 1.52 mmol) in tetrahydrofuran (2 ml) and then hexamethylphosphoric triamide (555 μl, 3.19 mmol) were dropwise added at -78° C. to a solution comprising 2.0M lithium diisopropylamide--tetrahydrofuran (1.6 ml, 3.19 mmol) and tetrahydrofuran (10 ml). The mixture was stirred at -78° C. for 30 minutes. Then, a solution of (2S,4R)-N-tert-butoxycarbonyl-4-tert-butyldimethylsiloxyprolinal (500 mg, 1.52 mmol) in tetrahydrofuran (2 ml) was dropwise added. The reaction mixture was stirred at room temperature for 2 h. Water was added to the reaction mixture. Then, the reaction mixture was poured into a mixture of ethyl acetate-water. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained oily residue was subjected to silica gel column chromatography (chloroform--methanol=20:1) to give the title compound (158 mg, yield: 25.9%).

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 2 h
  2. washThe organic layer was washed with saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1a583f2c104e472e8c9468e673d17c71
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…

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