Chlorotrimethylsilane → 3,9-Dioxa-2,10-disilaundecane, 2,2,10,10-tetramethyl-

HRID 5056

反応式

HRID 5056 の反応式
[CH2:1]([OH:7])[CH2:2][CH2:3][CH2:4][CH2:5][OH:6].[CH3:8][Si:9](Cl)([CH3:11])[CH3:10]>C[Si](N[Si](C)(C)C)(C)C>[Si:9]([O:6][CH2:5][CH2:4][CH2:3][CH2:2][CH2:1][O:7][Si:9]([CH3:11])([CH3:10])[CH3:8])([CH3:11])([CH3:10])[CH3:8]

参加物

4

反応物 2

HCID 6397ChlorotrimethylsilaneHCID 81051,5-Pentanediol

生成物 1

HCID 1431753,9-Dioxa-2,10-disilaundecane, 2,2,10,10-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

1,5-Pentanediol (65 g, 0.62 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.4 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 (130 mL, 0.71 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. (1 h), and 150° C. (2.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 139 g of colorless oil, bp 47°-49° C./0.1 mm. 1H NMR (CDCl3): 3.60 (t, J=7Hz, 4H), 1.57 (m, 4H), 1.40 (m, 2H), 0.12 (s, 18H), consistent with the assigned structure.

後処理

  1. customan exothermic reaction
  2. temperatureHeating
  3. customwas continued at 100° C.
  4. custom(1 h), and 150° C. (2.5 h)
  5. distillationDistillation

出典と根拠

ORDレコード
ord-8970a9cd79a34b338559a5f59227a0d1
出典データセット
uspto-grants-1993_09
特許番号
US05243025

関連ノート

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