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

HRID 1740329

反応式

HRID 1740329 の反応式
[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]

参加物

4

反応物 2

HCID 6397ChlorotrimethylsilaneHCID 80641,4-Butanediol

生成物 1

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

試薬・触媒・溶媒 1

HCID 13838Hexamethyldisilazane溶媒3 回

反応条件

温度
50 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-156f5532406741a79fc99e6874df5d47
出典データセット
uspto-grants-1999_10
特許番号
US05969074

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