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

HRID 897068
ノート
印刷プレビュー

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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 851405-Bromopentyl acetateHCID 107793113-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol

生成物 1

HCID 222527755-(3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)pentyl Acetate

試薬・触媒・溶媒 2

HCID 6569
Methyl Ethyl Ketone
溶媒
HCID 8857Ethyl Acetate溶媒

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
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06921777B2

反応ノート

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