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

HRID 850128ノート

反応式

HRID 850128 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3ab94c12469443d7acbbcb2807abbccd
出典データセット
uspto-grants-2000_01
特許番号
US06015868

反応ノート

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