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Tetramethoxysilane → 2-(Trimethoxysilyl)thianthrene

HRID 716587
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HRID 716587 반응식
[Mg].[CH3:2][O:3][Si:4](OC)([O:7][CH3:8])[O:5][CH3:6].Br[C:12]1[CH:25]=[CH:24][C:23]2[S:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[S:15][C:14]=2[CH:13]=1>C1COCC1>[CH3:2][O:3][Si:4]([O:7][CH3:8])([O:5][CH3:6])[C:12]1[CH:25]=[CH:24][C:23]2[S:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[S:15][C:14]=2[CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 12682TetramethoxysilaneHCID 5462224MagnesiumHCID 132131222-Bromothianthrene

생성물 1

HCID 711166972-(Trimethoxysilyl)thianthrene수율 60%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 3-neck 1 L flask was filled with magnesium turnings (5 g), THF (200 g) and tetramethoxysilane (50 g), and heated to reflux. 2-Bromothianthrene (40 g), prepared analogously to Example 3A was added to the flask in 10 g portions. Grignard started within 10 minutes. The reaction was allowed to cool for 1 hour, after which magnesium salts were precipitated with hexanes (200 mL). GC/MS of the solution showed that along with some thianthrene, 2-(trimethoxysilyl)thianthrene was obtained in ˜60% yield (FIG. 7).

후처리

  1. temperatureheated to reflux
  2. additionwas added to the flask in 10 g portions
  3. temperatureto cool for 1 hour
  4. customafter which magnesium salts were precipitated with hexanes (200 mL)

출처 및 근거

ORD 기록
ord-c3be22e915f540efa35b32c846145ac7
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09190616B2

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