BIS(TRIETHOXYSILYL)METHANE → HCID 178506912, 화합물

HRID 1061478노트

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HRID 1061478 반응식
[CH2:1]([O:3][Si:4]([CH2:11][Si:12]([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2].C([Li:26])(C)(C)C>>[CH2:17]([O:16][Si:12]([CH:11]([Li:26])[Si:4]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:3][CH2:1][CH3:2])([O:19][CH2:20][CH3:21])[O:13][CH2:14][CH3:15])[CH3:18]

참가 물질

3

반응물 2

HCID 9798044BIS(TRIETHOXYSILYL)METHANE2회HCID 178418306HCID 178418306, 화합물

생성물 1

HCID 178506912HCID 178506912, 화합물

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온도
-78 °C

실험 절차

A commercially available bis(triethoxysilyl)methane (BTM) was lithiated by the following procedure. To 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask attached to a bubbler was added 3.07 g (9.00 mmol) BTM and the solution was flushed for 5 minutes with nitrogen that had been passed through a drying column packed with CaCl2 and Drierite. The solution was cooled down to −78° C. and then 5.2 mL, 1.7 M (9 mmol) of t-butyllithium was added dropwise over 10 minutes. The solution was stirred for 30 minutes at −78° C. after which a very, faint yellowish solution resulted. Then the temperature of the solution was raised to room temperature (RT) and stirring continued for 30 minutes at RT after which the solution turned colorless.

후처리

  1. distillationTo 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask
  2. customthe solution was flushed for 5 minutes with nitrogen that
  3. customresulted
  4. temperatureThen the temperature of the solution was raised to room temperature (RT)
  5. stirringstirring
  6. waitcontinued for 30 minutes at RT

출처 및 근거

ORD 기록
ord-56ec9beedeac474d9ecb0826c96b1080
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960551B2

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