Water → HCID 19914920, 화합물

HRID 1650281노트

반응식

HRID 1650281 반응식
[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

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 19914911HCID 19914911, 화합물

생성물 1

HCID 19914920HCID 19914920, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-715f83ca5e014700aa390cfc906cff5c
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04923857

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