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

HRID 17782
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HRID 17782 반응식
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
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참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매
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HCID 962
Water
용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bd67b92e946446cd96d7efddfc3592d5
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07741245B2

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