Water → HCID 19914920、化合物

HRID 1090509ノート

反応式

HRID 1090509 の反応式
[CH2:1]([N:8]1[CH:12]([CH2:13][OH:14])[CH2:11][CH2:10][CH:9]1[CH2:15][O:16][Si:17]([C:20]([CH3:23])([CH3:22])[CH3:21])([CH3:19])[CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:26]I.O>O1CCCC1.C(OCC)(=O)C>[CH2:1]([N:8]1[CH:12]([CH2:13][O:14][CH3:26])[CH2:11][CH2:10][CH:9]1[CH2:15][O:16][Si:17]([C:20]([CH3:23])([CH3:22])[CH3:21])([CH3:18])[CH3:19])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 19914911HCID 19914911、化合物

生成物 1

HCID 19914920HCID 19914920、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-benzyl-2-t-butyldimethylsilyloxymethyl-5-hydroxymethylpyrrolidine (10 g) in tetrahydrofuran (100 ml) was added portionwise sodium hydride (2.3 g) at 0° C. The mixture was stirred at the same temperature for 30 minutes. And then methyl iodide was added to the mixture. After stirring for an hour at room temperature, water and ethyl acetate was added thereto. The aqueous layer was separated and washed twice with ethyl acetate. The combined organic layer was washed with saturated aqueous sodium hydrogen carbonate, water and brine successively, dried over magnesium sulfate and evaporated under reduced pressure to give 1-benzyl-2-t-butyldimethylsilyloxymethyl-5-methoxymethylpyrrolidine (9.99 g).

後処理

  1. stirringAfter stirring for an hour at room temperature
  2. customThe aqueous layer was separated
  3. washwashed twice with ethyl acetate
  4. washThe combined organic layer was washed with saturated aqueous sodium hydrogen carbonate, water and brine successively
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-2f868a9a7809472e908215f40a82b692
出典データセット
uspto-grants-1992_01
特許番号
US05081237

反応ノート

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