Butyl Chloride → N-butyl-4-amino-3,3-dimethylbutyltrimethoxysilane

HRID 1531332ノート

反応式

HRID 1531332 の反応式
[NH2:1][CH2:2][C:3]([CH3:14])([CH3:13])[CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:9][CH3:10])[O:7][CH3:8].Cl[CH2:16][CH2:17][CH2:18][CH3:19].C[O-].[Na+]>CO>[CH2:16]([NH:1][CH2:2][C:3]([CH3:14])([CH3:13])[CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:7][CH3:8])[O:9][CH3:10])[CH2:17][CH2:18][CH3:19]

参加物

5

反応物 3

HCID 8005Butyl Chloride2 回HCID 10942334Sodium MethoxideHCID 219390334-Amino-3,3-dimethylbutyltrimethoxysilane2 回

生成物 1

HCID 21253656N-butyl-4-amino-3,3-dimethylbutyltrimethoxysilane収率 77.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
125 °C

実験手順

In a 1 liter 3-necked flask equipped with a magnetic stirrer, heating mantle thermometers and condenser was added 664.1 g (3 moles) of 4-amino-3,3-dimethylbutyltrimethoxysilane and 69.4 g (0.75 mole) of 1-chlorobutane. With stirring, the flask contents were slowly heated to 125° C. and maintained at that temperature for a total of 13 hours. A gas chromatograph of a sample of the flask contents at that point indicated all of the chlorobutane had been consumed in the reaction with the aminofunctional silane. The flask was cooled to room temperature and 162 g of a 25% solution of sodium methoxide in methanol (0.75 mole of sodium methoxide) was added drop-wise by means of an addition funnel. After stirring for 30 minutes the flask contents were pressure filtered and distilled, yielding after removal of methanol and excess 4-amino-3,3-dimethylbutyltrimethoxysilane, 160.7 g of N-butyl-4-amino-3,3-dimethylbutyltrimethoxysilane (bp 90-94° C. at 1 mm Hg, 58% yield). The structure was confirmed by gc-mass spectroscopy and 1H and 13C nmr spectroscopy.

後処理

  1. customIn a 1 liter 3-necked flask equipped with a magnetic stirrer
  2. temperatureheating mantle thermometers and condenser
  3. temperaturemaintained at that temperature for a total of 13 hours
  4. customhad been consumed in the reaction with the aminofunctional silane
  5. temperatureThe flask was cooled to room temperature
  6. stirringAfter stirring for 30 minutes the flask contents
  7. filtrationfiltered
  8. distillationdistilled
  9. customyielding

出典と根拠

ORDレコード
ord-63625f56bf4649108ec24eada73f55d2
出典データセット
uspto-grants-2001_03
特許番号
US06197912B1

反応ノート

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