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Neopentyl glycol → 2-(4-Bromophenyl)-2-(3-chloropropyl)-5,5-dimethyl-1,3-dioxane

HRID 747710
ノート
印刷プレビュー

反応式

HRID 747710 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH2:9][CH2:10][CH2:11][Cl:12])=[CH:4][CH:3]=1.[CH3:14][C:15]([CH3:20])([CH2:18]O)[CH2:16][OH:17].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])O.[Na+]>C1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([CH2:9][CH2:10][CH2:11][Cl:12])[O:17][CH2:16][C:15]([CH3:20])([CH3:18])[CH2:14][O:13]2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 31344Neopentyl glycolHCID 783174'-Bromo-4-chlorobutyrophenoneHCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 126147752-(4-Bromophenyl)-2-(3-chloropropyl)-5,5-dimethyl-1,3-dioxane

試薬・触媒・溶媒 1

HCID 241Benzene
溶媒

実験手順

10 g (38.2 mmol) of 4′-bromo-4-chlorobutyrophenone, 4 g (38.2 mmol) of 2,2-dimethyl-1,3-propanediol and 200 mg (1 mmol) of p-toluenesulfonic acid monohydrate were heated under reflex in benzene for 3 days to conduct the azeotropic dehydration. Saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture. After the extraction with ethyl acetate, the extract was washed with water and saturated aqueous common salt solution and then dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the title compound.

後処理

  1. extractionAfter the extraction with ethyl acetate
  2. washthe extract was washed with water and saturated aqueous common salt solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-01cf6374aaa0467c886a41fd7ca1e808
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07396844B1

反応ノート

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