Dichlorodimethylsilane → HCID 59735669, 화합물

HRID 2425313노트

반응식

HRID 2425313 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

HCID 59735669HCID 59735669, 화합물

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f07651d63e64255823baeb08801fae1
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07964679B2

반응 노트

불러오는 중…