Propylene Glycol → 2,2,4,7,7-Pentamethyl-3,6-dioxa-2,7-disilaoctane

HRID 1740331

반응식

HRID 1740331 반응식
[CH2:1]([OH:5])[CH:2]([OH:4])[CH3:3].[CH3:6][Si:7](Cl)([CH3:9])[CH3:8]>C[Si](N[Si](C)(C)C)(C)C>[Si:7]([O:4][CH:2]([CH2:1][O:5][Si:7]([CH3:9])([CH3:8])[CH3:6])[CH3:3])([CH3:9])([CH3:8])[CH3:6]

참가 물질

4

반응물 2

HCID 1030Propylene GlycolHCID 6397Chlorotrimethylsilane

생성물 1

HCID 5194882,2,4,7,7-Pentamethyl-3,6-dioxa-2,7-disilaoctane

시약·촉매·용매 1

HCID 13838Hexamethyldisilazane용매3회

반응 조건

온도
60 °C

실험 절차

1,2-Propanediol (58.8 g, 0.77 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.2 mL trimethylsilyl chloride. A small volume of HMDS (ca. 10 mL) was added, and an exothermic reaction took place as the mixture became homogeneous. The remainder of the HMDS (170 mL) was added at a controlled rate (ca. 3-5 mL/min), maintaining the reaction temperature at ca. 50-70° C. Heating was continued at 100° C. (1.5 h), 120° C. (1.0 h), and 140° C. (2.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 147 g of colorless oil, bp 70-72° C./10 mm. 1H NMR (CDCl3): 3.83 (m, 1 H), 3.50 and 3.38 (AB pattern with additional coupling, 2 H), 1.15 (d, J=7 Hz, 3 H), 0.15 (partially resolved singlets, 18 H).

후처리

  1. customan exothermic reaction
  2. temperatureHeating
  3. customwas continued at 100° C.
  4. custom(1.5 h), 120° C. (1.0 h), and 140° C. (2.5 h)
  5. distillationDistillation

출처 및 근거

ORD 기록
ord-04e69c0abac141f3a57b0b8246c89750
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05969074

연결된 노트

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