Dimethylformamide → 4-(4-Bromobutyl)-2,2-dimethyl-1,3-dioxolane

HRID 1577695노트

반응식

HRID 1577695 반응식
[CH3:1][C:2]1([CH3:22])[O:6][CH:5]([CH2:7][CH2:8][CH2:9][CH2:10]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:4][O:3]1.CN(C)C=O.[Br-:28].[Li+]>O>[Br:28][CH2:10][CH2:9][CH2:8][CH2:7][CH:5]1[CH2:4][O:3][C:2]([CH3:22])([CH3:1])[O:6]1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 82050Lithium BromideHCID 127708652,2-Dimethyl-4-(4-p-toluenesulfonyloxybutyl)-1,3-dioxolane

생성물 1

HCID 46572524-(4-Bromobutyl)-2,2-dimethyl-1,3-dioxolane

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 220 g. of 2,2-dimethyl-4-(4-p-toluenesulfonyloxybutyl)-1,3-dioxolane in 800 ml. of dimethylformamide at 0° C. is added 115 g. of anhydrous lithium bromide in portions during 5 minutes. The resulting mixture is stirred at ambient temperature for 22 hours, diluted with water, and extracted with ether. The extract is washed with sodium bicarbonate solution, water, and brine; dried over magnesium sulfate; and concentrated. The residue is distilled to give a colorless liquid, b.p. 71°-74° C. (0.2 mm.).

후처리

  1. extractionextracted with ether
  2. washThe extract is washed with sodium bicarbonate solution, water, and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationand concentrated
  5. distillationThe residue is distilled
  6. customto give a colorless liquid, b.p. 71°-74° C. (0.2 mm.)

출처 및 근거

ORD 기록
ord-5d0e834004b8468080fd7cac9fc82160
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04288633

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