Chlorotrimethylsilane → 3,8-Dioxa-2,9-disiladecane, 2,2,9,9-tetramethyl-

HRID 1740329

반응식

HRID 1740329 반응식
[CH2:1]([OH:6])[CH2:2][CH2:3][CH2:4][OH:5].[CH3:7][Si:8](Cl)([CH3:10])[CH3:9]>C[Si](N[Si](C)(C)C)(C)C>[Si:8]([O:5][CH2:4][CH2:3][CH2:2][CH2:1][O:6][Si:8]([CH3:10])([CH3:9])[CH3:7])([CH3:10])([CH3:9])[CH3:7]

참가 물질

4

반응물 2

HCID 6397ChlorotrimethylsilaneHCID 80641,4-Butanediol

생성물 1

HCID 1403213,8-Dioxa-2,9-disiladecane, 2,2,9,9-tetramethyl-

시약·촉매·용매 1

HCID 13838Hexamethyldisilazane용매3회

반응 조건

온도
50 °C

실험 절차

1,4-Butanediol (54 g, 0.60 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.3 mL trimethylsilyl chloride. A portion of HMDS (ca. 20 mL) was added, and an exothermic reaction took place as the mixture became homogeneous. The remainder of the HMDS (120 mL, 0.66 mol total) was added at a controlled rate (ca. 3-5 mL/min), maintaining the reaction temperature at ca. 50° C. Heating was continued at 100° C. (3 h), and 150° C. (1.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 127.8 g of colorless oil, bp 97-99° C./15 mm. 1H NMR (CDCl3): 3.75-3.50 (m, 4 H), 1.75-1.50 (m, 4 H), 0.16 (s, 18 H).

후처리

  1. customan exothermic reaction
  2. temperatureHeating
  3. customwas continued at 100° C.
  4. custom(3 h), and 150° C. (1.5 h)
  5. distillationDistillation

출처 및 근거

ORD 기록
ord-156f5532406741a79fc99e6874df5d47
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05969074

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