Imidazole → Hexaethyldisiloxane

HRID 1870589노트

반응식

HRID 1870589 반응식
N1[CH:5]=[CH:4]N=C1.[CH2:6]([Si:8](Cl)([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7].[OH2:14]>CN(C)C=O>[CH2:6]([Si:8]([O:14][Si:8]([CH2:4][CH3:5])([CH2:9][CH3:10])[CH2:6][CH3:7])([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7]

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 962WaterHCID 13819Chlorotriethylsilane

생성물 1

HCID 70442Hexaethyldisiloxane

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 205 (15 mmol) in dimethylformamide (30 mL) is cooled to 0° C. and treated with imidazole (30 mmol) and triethylsilyl chloride (20 mmol). The resultant solution is warmed to room temperature. After 12 h, the reaction mixture is poured into 300 mL of water and extracted with ether (3×40 mL). The ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL), dried over magnesium sulfate and concentrated in vacuo. The residue is purified by flash chromatography to afford 206.

후처리

  1. extractionextracted with ether (3×40 mL)
  2. washThe ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL)
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by flash chromatography

출처 및 근거

ORD 기록
ord-9c5e481612374ec59d0b2557dd10087c
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06096904

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