Chloro(1H-inden-2-yl)dimethylsilane → HCID 21195280, 화합물

HRID 1068060노트

반응식

HRID 1068060 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Li].Cl[Si:16]([C:19]1[CH2:20][C:21]2[C:26]([CH:27]=1)=[CH:25][CH:24]=[CH:23][CH:22]=2)([CH3:18])[CH3:17]>C(OCC)C>[C:1]1([Si:16]([C:19]2[CH2:20][C:21]3[C:26]([CH:27]=2)=[CH:25][CH:24]=[CH:23][CH:22]=3)([CH3:17])[CH3:18])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 22395124Chloro(1H-inden-2-yl)dimethylsilaneHCID 69882698Lithium Fluorene

생성물 1

HCID 21195280HCID 21195280, 화합물수율 75%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
25 °C

실험 절차

A solution of lithium fluorene from Example 4 was slowly added dropwise at 0° C., by means of a septum and a syringe, to a solution of chloro-2-indenyl-dimethylsilane (2.85 g, 0.0136 mol.) according to Example 1 in 20 ml of diethyl ether. After 2 hours' stirring at 25° C., the resulting LiCl was filtered off. The solvent was removed from the filtrate and the beige-colored residue was dissolved in hot ether/petroleum ether and crystallized at −30° C. 3.45 g (75%) of fluorenyl-2-indenyldimethylsilane were obtained in the form of a colorless solid. M.p.: 125° C.

후처리

  1. filtrationthe resulting LiCl was filtered off
  2. customThe solvent was removed from the filtrate
  3. dissolutionthe beige-colored residue was dissolved in hot ether/petroleum ether
  4. customcrystallized at −30° C

출처 및 근거

ORD 기록
ord-746a1a14c18e4d4594212a98fb5e6d7a
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248912B1

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