Dichlorodimethylsilane → HCID 59735669、化合物

HRID 2425313ノート

反応式

HRID 2425313 の反応式
[Li]CCCC.[CH3:6][C:7]1[CH2:8][C:9]2[C:14]([CH:15]=1)=[C:13]([CH3:16])[CH:12]=[C:11]([CH3:17])[CH:10]=2.[Si:18]([CH3:22])([CH3:21])(Cl)[Cl:19].[Li]>CCCCCC.CCOCC.C1COCC1>[Cl:19][Si:18]([CH:8]1[C:9]2[C:14](=[C:13]([CH3:16])[CH:12]=[C:11]([CH3:17])[CH:10]=2)[CH:15]=[C:7]1[CH3:6])([CH3:22])[CH3:21]

参加物

8

反応物 4

HCID 6398DichlorodimethylsilaneHCID 3028194LithiumHCID 109207862,4,6-trimethyl-1H-indeneHCID 178418339Butyllithium

生成物 1

HCID 59735669HCID 59735669、化合物

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

実験手順

A 2.5 M n-BuLi solution in hexane (9.6 mL) was added dropwise at 0° C. under nitrogen to a solution of 3.6 g of 2,4,6-trimethylindene in 35 mL of Et2O. During the addition a white-off suspension was formed. After 10 min the mixture was allowed to warm up to r.t. and stirred for 30 min, with final formation of a white suspension. Then a solution of Me2SiCl2 (4 mL) in 35 mL of THF was cooled to 0° C. and slowly added to the lithium salt suspension, also cooled to 0° C. After 30 min the yellow reaction mixture was allowed to warm up to r.t. and stirred for 24 h. Then the solvents were removed in vacuo and the light orange oil with a powder was characterized by 1H-NMR spectroscopy. The product was used as such in the next step without further purification.

後処理

  1. additionDuring the addition a white-off suspension
  2. customwas formed
  3. temperaturealso cooled to 0° C
  4. waitAfter 30 min the yellow reaction mixture was allowed
  5. temperatureto warm up to r.t.
  6. stirringstirred for 24 h
  7. customThen the solvents were removed in vacuo
  8. customwithout further purification

出典と根拠

ORDレコード
ord-2f07651d63e64255823baeb08801fae1
出典データセット
uspto-grants-2011_06
特許番号
US07964679B2

反応ノート

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