Triethylamine → 4-(6-Methacryloxyhexyloxy)-4'-nitrobiphenyl

HRID 2082113Notes

Reaction equation

[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)=[CH:11][CH:10]=1.C(N(CC)CC)C.[C:31](Cl)(=[O:35])[C:32]([CH3:34])=[CH2:33]>O1CCOCC1>[C:31]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]([N+:21]([O-:23])=[O:22])=[CH:19][CH:20]=2)=[CH:11][CH:10]=1)(=[O:35])[C:32]([CH3:34])=[CH2:33]

Participants

Conditions

Temperature: 45 °C

Procedure

77 g 4-(6-hydroxyhexyloxy)-4'-nitrobiphenyl (see Example 4) is dissolved in 1500 ml absolute dioxane, and the solution is then heated to 45° C. Subsequently, 26.8 g triethylamine and 27.2 g methacrylic acid chloride, dissolved in the same volume of dioxane, are dripped in, then the reaction mixture is stirred for 24 h. Subsequently, the solvent is removed in a vacuum and the reaction mixture is suspended in water; the solid is filtered off, washed with water, dried and recrystallized from ethanol (melting point: 57° C.); yield: 80%.

Workup

customSubsequently, the solvent is removed in a vacuum
filtrationthe solid is filtered off
washwashed with water
customdried
customrecrystallized from ethanol (melting point: 57° C.)

Sources & evidence

ORD record: ord-64262c3c884f4f76a4efc1a10cd0d6af
Source dataset: uspto-grants-1993_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05187237

Reaction notes

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