Benzylamine → N-[(Trimethylsilyl)methyl]benzylamine

HRID 374255

반응식

HRID 374255 반응식
Cl[CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4].[CH2:7]([NH2:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>>[CH2:7]([NH:14][CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

4

반응물 3

HCID 7504BenzylamineHCID 11430Potassium CarbonateHCID 75361Silane, (chloromethyl)trimethyl-

생성물 1

HCID 353458N-[(Trimethylsilyl)methyl]benzylamine

반응 조건

온도
120 °C

실험 절차

A mixture of chloromethyltrimethylsilane (325g, 370 ml, 2.65 mole) and benzylamine (835 g, 850 ml, 7.78 mole) was heated at 120° C. (oil bath temperature) for 2 h. A white solid began appearing after only 10 minutes and a viscous mixture eventually resulted. The reaction mixture was allowed to cool, then basified with potassium carbonate solution and extracted twice with ether. The combined extracts were dried (Na2SO4) and concentrated in vacuo to leave a yellow oil, which was purified by distillation. The excess benzylamine was removed in the first fractions (b.p. 47°-62° C. at 2 mmHg). The title compound (D10) was obtained as a colourless oil (380 g, 74%) b.p. 75°-80° C. at 2 mmHg.

후처리

  1. customa viscous mixture eventually resulted
  2. temperatureto cool
  3. extractionextracted twice with ether
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customto leave a yellow oil, which
  7. distillationwas purified by distillation
  8. customThe excess benzylamine was removed in the first fractions (b.p. 47°-62° C. at 2 mmHg)

출처 및 근거

ORD 기록
ord-c3e2d58493ae4b80a2f18d2a5f6e8769
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166357

연결된 노트

불러오는 중…