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

HRID 1531332노트

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HRID 1531332 반응식
[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]

참가 물질

5

반응물 3

HCID 8005Butyl Chloride2회HCID 10942334Sodium MethoxideHCID 219390334-Amino-3,3-dimethylbutyltrimethoxysilane2회

생성물 1

HCID 21253656N-butyl-4-amino-3,3-dimethylbutyltrimethoxysilane수율 77.2%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
125 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-63625f56bf4649108ec24eada73f55d2
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197912B1

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