2-Methyl-4-phenylindene → (2-Methyl-4-phenylindenyl)(t-butylamino)dimethylsilane

HRID 850128노트

반응식

HRID 850128 반응식
[CH3:1][C:2]1[CH2:3][C:4]2[C:9]([CH:10]=1)=[C:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH:7]=[CH:6][CH:5]=2.[CH3:17][SiH:18]([N:20](Cl)[C:21]([CH3:24])([CH3:23])[CH3:22])[CH3:19]>C1COCC1>[CH3:1][C:2]1[CH:3]([Si:18]([NH:20][C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:19])[CH3:17])[C:4]2[C:9]([CH:10]=1)=[C:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH:7]=[CH:6][CH:5]=2

참가 물질

4

반응물 2

HCID 110745592-Methyl-4-phenylindeneHCID 123286153Dimethylsilyl(t-butylamino)chloride

생성물 1

HCID 19366102(2-Methyl-4-phenylindenyl)(t-butylamino)dimethylsilane수율 82%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

2-methyl-4-phenylindene (synthesized substantially according to the technique reported in U.S. Pat. No. 5,329.033) (3.00 g, 0.014 moles) in THF (10 mL) was added dropwise to a stirring solution of KH (0.601 g, 0.0150 moles) in THF (50 mL). This mixture was allowed to stir for 16 hours. The solution was then filtered and added dropwise to a solution of dimethylsilyl(t-butylamino)chloride (2.41 g, 0.0145 moles) in THF (75 mL). This mixture was allowed to stir for 16 hours. After the reaction period the volatiles were removed and the residue extracted and filtered using hexane. Removal of the volatiles resulted in the isolation of the desired product as a light yellow oil (4.00 g, 82.0 percent).

후처리

  1. filtrationThe solution was then filtered
  2. stirringto stir for 16 hours
  3. customAfter the reaction period the volatiles
  4. customwere removed
  5. extractionthe residue extracted
  6. filtrationfiltered
  7. customRemoval of the volatiles

출처 및 근거

ORD 기록
ord-3ab94c12469443d7acbbcb2807abbccd
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06015868

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