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Lithium → HCID 14908225、化合物

HRID 982535
ノート
印刷プレビュー

反応式

HRID 982535 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 14908225HCID 14908225、化合物収率 101.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f3aab6c1292245a18e978e8d5dd12949
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04996341

反応ノート

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