4-(Bromomethyl)-2,2-dimethyl-1,3-dioxolane → (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl benzoate

HRID 1857061

반응식

HRID 1857061 반응식
[C:1]([O-:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Na+].Br[CH2:12][CH:13]1[CH2:17][O:16][C:15]([CH3:19])([CH3:18])[O:14]1>CN(C)C=O>[C:1]([O:9][CH2:12][CH:13]1[CH2:17][O:16][C:15]([CH3:19])([CH3:18])[O:14]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 1697594-(Bromomethyl)-2,2-dimethyl-1,3-dioxolaneHCID 517055Sodium Benzoate

생성물 1

HCID 571151(2,2-Dimethyl-1,3-dioxolan-4-yl)methyl benzoate수율 91%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

Then, sodium benzoate (50.44 g, 0.35 mol) were added to a mixture of 4-bromomethyl-2,2-dimethyl-1,3-dioxolane (58.52 g, 0.3 mol) and N,N-dimethylformamide (500 ml) and the resulting mixture was stirred for 15 hours at 150° C. After cooling the salt was filtered and N,N-dimethylformamide was removed in vacuo and water was added to the residue and extracted with toluene. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and condensed in vacuo to give 64.5 g of crude 4-benzoyloxymethyl-2,2-dimethyl-1,3-dioxolane (yield 91%).

후처리

  1. temperatureAfter cooling the salt
  2. filtrationwas filtered
  3. customN,N-dimethylformamide was removed in vacuo and water
  4. additionwas added to the residue
  5. extractionextracted with toluene
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate and condensed in vacuo

출처 및 근거

ORD 기록
ord-b283fed5cf0f464faa6011368a0141de
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06143908

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