Hexane → HCID 21658117, compound

HRID 1276042Notes

Reaction equation

[CH2:1]([Si:5]([O:10][CH3:11])([O:8][CH3:9])[O:6][CH3:7])[CH2:2][CH2:3][CH3:4].[CH3:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>>[CH2:1]([Si:5]([O:10][CH3:11])([O:6][CH3:7])[O:8][CH3:9])[CH2:2][CH2:3][CH3:4].[CH3:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

Participants

Reactant 2

HCID 8058Hexane

HCID 70601Silane, butyltrimethoxy-

Product 1

HCID 21658117HCID 21658117, compound

Conditions

Temperature: 0 °C

Procedure

In a separate reaction vessel under nitrogen, 5.0 ml n-butyl(trimethoxy)silane (0.026 mol.) was added along with 50 ml hexane. The vessel was cooled to 0° C. in an ice bath while stirring. To the cooled n-butyl(trimethoxy)silane/hexane solution obtained was added, via cannula, 2.68 g 1-lithio-4-methylpiperidine suspension from the first vessel. After the addition was completed, the reaction mixture was allowed to warm to room temperature, stirred for about 16 hours, then heated to reflux for about 2 hours. The solvents were then removed in vacuo and the white solid was washed 3 times with 20 ml portions of hexane to remove the product. The hexane was stripped from the product under vacuum to give an oil.

Workup

customIn a separate reaction vessel under nitrogen

Sources & evidence

ORD record: ord-7edf235a55c14327b030e76c02ce7829
Source dataset: uspto-grants-2000_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06165930

Reaction notes

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