Water → 5-(3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)pentyl Acetate

HRID 897068

反応式

HRID 897068 の反応式
[Br:1][C:2]1[C:3]([OH:16])=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.[C:17]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]Br)(=[O:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+].O>C(C(C)=O)C.C(OCC)(=O)C>[C:17]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][O:16][C:3]1[C:2]([Br:1])=[CH:11][C:10]2[C:9]([CH3:12])([CH3:13])[CH2:8][CH2:7][C:6]([CH3:15])([CH3:14])[C:5]=2[CH:4]=1)(=[O:19])[CH3:18]

参加物

7

実験手順

A solution of 3-bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol (10 g, 0.35 mol), 5-bromopentyl acetate (8.15 g) and potassium carbonate (33.6 g) in methyl ethyl ketone (200 ml) is refluxed for 2 hours. The reaction medium is treated with water and ethyl acetate. After separation of the phases by settling, the organic phase is washed twice with water, dried over magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40° C. The product is purified by flash chromatography on a column of silica.

後処理

  1. customAfter separation of the phases
  2. washthe organic phase is washed twice with water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated on a rotary evaporator under vacuum at 40° C
  5. customThe product is purified by flash chromatography on a column of silica

出典と根拠

ORDレコード
ord-88a8d2ce6fd74a33a3f31ab483d92a26
出典データセット
uspto-grants-2005_07
特許番号
US06921777B2

関連ノート

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