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t-Butylaminodimethylsilylchloride → (N-t-butylamino)(dimethyl)(1,3-dimethyl-4,5,6,7-tetrahydroindenyl)silane

HRID 54889
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HRID 54889 반응식
Cl[Si:2]([NH:5][C:6]([CH3:9])([CH3:8])[CH3:7])([CH3:4])[CH3:3].[CH3:10][C-:11]1[C:19]2[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=2[C:13]([CH3:20])=[CH:12]1.[Li+]>C1COCC1>[C:6]([NH:5][Si:2]([CH3:4])([CH3:3])[C:12]1[CH:11]([CH3:10])[C:19]2[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=2[C:13]=1[CH3:20])([CH3:9])([CH3:8])[CH3:7]
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참가 물질

4

반응물 2

HCID 11205972t-ButylaminodimethylsilylchlorideHCID 23721395Lithium 1,3-dimethyl-4,5,6,7-tetrahydro-1H-inden-1-ide

생성물 1

HCID 19956842(N-t-butylamino)(dimethyl)(1,3-dimethyl-4,5,6,7-tetrahydroindenyl)silane수율 94%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In an argon atmosphere drybox 0.77 g of ClSiMe2NHCMe3 (4.67 mmol) was added to 50 mL of THF. To this solution 0.75 g (4.67 mmol) of lithium 1,3-dimethyl-4,5,6,7-tetrahydroindenide was added. The solution was then brought to reflux for about 3 hours and then cooled to room temperature. Chromatographic analysis showed the reaction to be complete. The solvent was then removed under reduced pressure. The residue was extracted with pentane, filtered, and the solvent again removed under reduced pressure to give 1.21 g of product (94 percent yield).

후처리

  1. temperatureto reflux for about 3 hours
  2. customthe reaction
  3. customThe solvent was then removed under reduced pressure
  4. extractionThe residue was extracted with pentane
  5. filtrationfiltered
  6. customthe solvent again removed under reduced pressure

출처 및 근거

ORD 기록
ord-fc33ceef87d64de19b8cde6c7272608b
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05624878

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