Benzene → 2,2-Bis-chloromethyl-5,5-dimethyl-1,3-dioxolane

HRID 17782

反応式

HRID 17782 の反応式
OC[C:3]([CH3:7])([CH2:5][OH:6])[CH3:4].[Cl:8][CH2:9][C:10]([CH2:12][Cl:13])=[O:11].C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>C1(C)C=CC(S(O)(=O)=O)=CC=1.O>[Cl:8][CH2:9][C:10]1([CH2:12][Cl:13])[O:6][CH2:5][C:3]([CH3:4])([CH3:7])[O:11]1

参加物

7

反応物 4

HCID 241BenzeneHCID 107931,3-DichloroacetoneHCID 31344Neopentyl glycolHCID 516892Sodium Bicarbonate

生成物 1

HCID 685854382,2-Bis-chloromethyl-5,5-dimethyl-1,3-dioxolane収率 34.6%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 962Water溶媒

実験手順

This compound was synthesized by substantially following the procedure of the above-mentioned article by Isaka, Ejiri, and Nakamura. 69 grams of neopentyl glycol, 76 grams of 1,3-dichloroacetone, 50 ml of benzene, and 2.3 g of p-toluenesulfonic acid were refluxed through a Dean-Stark water separator for 8 hours whereon the reaction was diluted with hexanes and neutralized with aqueous sodium bicarbonate. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo yielding 41.2 g of 2,2-bis-chloromethyl-5,5-dimethyl-1,3-dioxolane, a pale yellow liquid.

後処理

  1. customThis compound was synthesized
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bd67b92e946446cd96d7efddfc3592d5
出典データセット
uspto-grants-2010_06
特許番号
US07741245B2

関連ノート

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