BIS(TRIETHOXYSILYL)METHANE → HCID 178506912、化合物

HRID 1061478ノート

反応式

HRID 1061478 の反応式
[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]

参加物

3

反応物 2

HCID 9798044BIS(TRIETHOXYSILYL)METHANE2 回HCID 178418306HCID 178418306、化合物

生成物 1

HCID 178506912HCID 178506912、化合物

反応条件

温度
-78 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-56ec9beedeac474d9ecb0826c96b1080
出典データセット
uspto-grants-2005_11
特許番号
US06960551B2

反応ノート

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