N,N-Dimethylaniline → gamma-Diethoxymethylsilylpropyl isocyanate

HRID 1906975

반응식

HRID 1906975 반응식
[C:1](Cl)(Cl)=[O:2].[CH2:5]([O:7][CH:8]([SiH2:12][CH2:13][CH2:14][CH2:15][NH2:16])[O:9][CH2:10][CH3:11])[CH3:6].CN(C)C1C=CC=CC=1.Cl.CN(C)C1C=CC=CC=1>C1(C)C=CC=CC=1>[CH2:10]([O:9][CH:8]([SiH2:12][CH2:13][CH2:14][CH2:15][N:16]=[C:1]=[O:2])[O:7][CH2:5][CH3:6])[CH3:11]

참가 물질

6

반응물 4

HCID 949N,N-DimethylanilineHCID 6371PhosgeneHCID 79987Benzenamine, N,N-dimethyl-, hydrochloride (1:1)HCID 573711433-(Diethoxymethylsilyl)propan-1-amine

생성물 1

HCID 123303072gamma-Diethoxymethylsilylpropyl isocyanate수율 71.9%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

In 150 ml of toluene was dissolved 9.9 g of carbonyl chloride, and a solution of 19.1 g of γ-diethoxymethylsilylpropylamine and 24.2 g of N,N-dimethylaniline in 50 ml of toluene was dropped into the above solution at -5° C. to -10° C. over a period of 3 hours to effect reaction. After the reaction, N,N-dimethylaniline hydrochloride was removed by filtration, the filtrate was distilled to recover toluene, and a fraction having a boiling point of 91° C. to 93° C. under 9 mmHg was collected. Then, 1 g of sodium benzoate was added to the fraction. The mixture was then stirred for 3 hours and the pH value became 7. Excessive sodium benzoate and the precipitate were removed by filtration, and the filtrate was distilled to obtain 15.6 g of γ-diethoxymethylsilylpropyl isocyanate as a fraction having a boiling point of 80° C. to 82° C. under 5 mmHg. The product remained stable, even when stored for more than 6 months.

후처리

  1. customreaction
  2. customwas removed by filtration
  3. distillationthe filtrate was distilled
  4. customto recover toluene
  5. customwas collected
  6. additionThen, 1 g of sodium benzoate was added to the fraction
  7. customExcessive sodium benzoate and the precipitate were removed by filtration
  8. distillationthe filtrate was distilled

출처 및 근거

ORD 기록
ord-269ac2c2404443aca8d54cb1bcdd30ec
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04654428

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