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

HRID 1105988ノート

反応式

HRID 1105988 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-337e225467e242daaf6b7c2fec5def88
出典データセット
uspto-grants-1982_01
特許番号
US04310700

反応ノート

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