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Lithium → HCID 14908225, 화합물

HRID 982535
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HRID 982535 반응식
[Li].[C:2]1([Si:8]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)([CH:10]([CH3:12])[CH3:11])Cl)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C1COCC1>[CH:10]([Si:8]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[Si:8]([CH:10]([CH3:12])[CH3:11])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)([CH3:12])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3028194LithiumHCID 12600818Chloro(diphenyl)(propan-2-yl)silane

생성물 1

HCID 14908225HCID 14908225, 화합물수율 101.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 1 liter three necked flask was charged with 200 ml of dry THF and then 5.04 g (0.73 mole) of small pieces of lithium metal was quickly added. To this was added dropwise 155 g of diphenylisopropylchlorosilane (purity: 94% by weight, 0.56 mole) at a room temperature over 2 hours. A mildly exothermic reaction was observed. After the dropwise addition, the reaction mixture was agitated for 3 days. The reaction mixture turned red purple. The formed salt and the solvent were removed from tho reaction mixture. To the residue was added about 300 ml of benzene, whereby the residue was dissolved therein. The benzene solution was washed with a saturated aqueous solution of ammonium chloride (300 ml×3 times) and then with water (300 ml×1 time) and dried over anhydrous magnesium sulfate. The drying agent was filtered off and the filtrate was concentrated to give 128 g of a crude product in a pale yellow solid.

후처리

  1. customA mildly exothermic reaction
  2. additionAfter the dropwise addition
  3. customThe formed salt and the solvent were removed from tho reaction mixture
  4. additionTo the residue was added about 300 ml of benzene, whereby the residue
  5. dissolutionwas dissolved
  6. washThe benzene solution was washed with a saturated aqueous solution of ammonium chloride (300 ml×3 times)
  7. dry with materialwith water (300 ml×1 time) and dried over anhydrous magnesium sulfate
  8. filtrationThe drying agent was filtered off
  9. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-f3aab6c1292245a18e978e8d5dd12949
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04996341

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