Dichloromethane → 4-Tert-butyldimethylsilyloxymethyl-2-allylphenol

HRID 257821

반응식

HRID 257821 반응식
C([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH2:9][OH:10])=[CH:7][CH:6]=1)C=C.C(N([CH2:18][CH3:19])CC)C.[Si:20](Cl)([C:23]([CH3:26])([CH3:25])[CH3:24])([CH3:22])[CH3:21].[CH2:28](Cl)Cl>C(OCC)(=O)C>[Si:20]([O:10][CH2:9][C:8]1[CH:7]=[CH:6][C:5]([OH:4])=[C:12]([CH2:28][CH:18]=[CH2:19])[CH:11]=1)([C:23]([CH3:26])([CH3:25])[CH3:24])([CH3:22])[CH3:21]

참가 물질

6

반응물 4

HCID 6344Dichloromethane2회HCID 8471TriethylamineHCID 28928tert-Butyldimethylsilyl chlorideHCID 11744970(4-(Prop-2-en-1-yloxy)phenyl)methanol

생성물 1

HCID 199348384-Tert-butyldimethylsilyloxymethyl-2-allylphenol

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the product of Step A (650 mg, 3.96 mmol) in CH2Cl2 (20 mL), cooled to 0° C. under nitrogen, was added triethylamine (612 mL, 4.39 mmol) and a solution of tert-butyldimethylsilyl chloride (631 mg; 4.19 mmol) in CH2Cl2 (2 mL). After stirring at room temperature for 18 hours, the reaction mixture was diluted with ethyl acetate (60 mL), washed with water, and saturated sodium bicarbonate, and then dried (MgSO4). The filtrate was concentrated in vacuo to afford 1.1 g of the title compound which was used crude in the next reaction (Rf =0.45, 5% ethyl acetate/hexanes).

후처리

  1. washwashed with water, and saturated sodium bicarbonate
  2. dry with materialdried (MgSO4)
  3. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-5d8d2590ded8469297d4eab6f0d4da32
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264439

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