1-Dodecene → Dichlorodidodecylsilane

HRID 1797765ノート

反応式

HRID 1797765 の反応式
[Cl:1][SiH2:2][Cl:3].[CH2:4]=[CH:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]>C(O)(C)C.O.Cl.Cl.Cl[Pt](Cl)(Cl)Cl>[Cl:1][Si:2]([Cl:3])([CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH3:4])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]

参加物

5

反応物 2

HCID 81831-DodeceneHCID 61330Dichlorosilane

生成物 1

HCID 21889369Dichlorodidodecylsilane

試薬・触媒・溶媒 2

HCID 16211507Platinate(2-), hexachloro-, hydrogen, hydrate (1:2:1), (OC-6-11)-触媒HCID 3776Isopropanol溶媒

反応条件

温度
0 °C

実験手順

To a dry tarred 500 mL Schlenk bomb flask was condensed 29.0 g (0.286 mol) of dichlorosilane at −78° C. To this was added 100 g (0.594 mol) of 1-dodecene under an argon flow. This mixture was allowed to warm to 0° C., then 100 mg (0.193 mmol) of hexachloroplatinic acid hexahydrate dissolved in 2 mL of isopropanol was added via syringe. The mixture was allowed to slowly warm to room temperature where it was allowed to stir for 40 hours. After this time the solution was cannula transferred into a dry 250 mL 3-necked round bottom flask equipped with a fractional distillation apparatus. The mixture was distilled at 220° C. at 0.1 mmHg. Yield: 78.1 g (62.5%). 1H NMR (400 MHz, C6D6): δ=1.6-1.4 (m, 4H), 1.4-1.1 (m, 36H), 1.0-0.8 (m, 10H). 13C NMR (100 MHz, C6D6): δ=33.19, 32.72, 30.51, 30.30, 30.21, 29.89, 23.51, 23.16, 20.92, 14.77. HRMS (EI) m/z, calcd for C24H50Cl2Si (M+): 436.3059; found: 436.3058.

後処理

  1. customTo a dry tarred 500 mL Schlenk bomb flask was
  2. additionwas added via syringe
  3. temperatureto slowly warm to room temperature where it
  4. customtransferred into a dry 250 mL 3-necked round bottom flask
  5. customequipped with a fractional distillation apparatus
  6. distillationThe mixture was distilled at 220° C. at 0.1 mmHg

出典と根拠

ORDレコード
ord-a479cd8cd4bf40a4823c0309ae2e79a7
出典データセット
uspto-grants-2013_01
特許番号
US08343382B2

反応ノート

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