1-Dodecene → Dichlorodidodecylsilane

HRID 1797765

반응식

HRID 1797765 반응식
[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]

참가 물질

5

반응물 2

HCID 81831-DodeceneHCID 61330Dichlorosilane

생성물 1

HCID 21889369Dichlorodidodecylsilane

시약·촉매·용매 2

HCID 16211507Platinate(2-), hexachloro-, hydrogen, hydrate (1:2:1), (OC-6-11)-촉매HCID 3776Isopropanol용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a479cd8cd4bf40a4823c0309ae2e79a7
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08343382B2

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