2,2,4,4,6,6,8,8-Octamethylcyclotetrasilazane → 2,2,4,4,6,6-Hexamethylcyclotrisilazane

HRID 1461563

반응식

HRID 1461563 반응식
C[Si]1(C)[NH:9][Si:8]([CH3:11])([CH3:10])[NH:7][Si:6]([CH3:13])([CH3:12])[NH:5][Si:4]([CH3:15])([CH3:14])N1>C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N[Si](C)(C)N1.NC1C=CC(C)=C(S(O)(=O)=O)C=1>[CH3:15][Si:4]1([CH3:14])[NH:5][Si:6]([CH3:12])([CH3:13])[NH:7][Si:8]([CH3:10])([CH3:11])[NH:9]1

참가 물질

4

반응물 1

HCID 661002,2,4,4,6,6,8,8-Octamethylcyclotetrasilazane

생성물 1

HCID 660942,2,4,4,6,6-Hexamethylcyclotrisilazane

시약·촉매·용매 2

HCID 661002,2,4,4,6,6,8,8-Octamethylcyclotetrasilazane촉매HCID 670545-Amino-2-methylbenzenesulfonic acid촉매

반응 조건

온도
97 °C

실험 절차

A 200 ml volume glass flask equipped with a stirring machine, a condenser, a distillation column and a tube for distilling off the resulting product was provided. 73 g of octamethyl cyclotetrasilazane and 3.65 g of p-toluidine-m-sulfonic acid as a catalyst were introduced into the glass flask and the content of the flask was heated to 97° C. The content of the flask was stirred after it was confirmed that the octamethyl cyclotetrasilazane was completely molten. When the internal pressure of the reaction system was reduced to 65 torr with a vacuum pump to obtain a distillate, 68 g of hexamethyl cyclotrisilazane was obtained through the distillation over one hour. The resulting hexamethyl cyclotrisilazane had a high purity in the order of 99.1 GC % and the yield thereof was 93.2%. Thus, highly pure hexamethyl cyclotrisilazane could be obtained at a high yield within a short period of time. Moreover, almost no high boiling point substance remained in the reaction system.

후처리

  1. customA 200 ml volume glass flask equipped with a stirring machine, a condenser
  2. distillationa distillation column and a tube
  3. distillationfor distilling off the resulting product
  4. customwas provided
  5. customto obtain a distillate

출처 및 근거

ORD 기록
ord-ac928fd5c76e4e48b2464afae04e1d3c
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075474

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