3-Chlorobenzoic Acid → Safrole oxide

HRID 461403

反応式

HRID 461403 の反応式
[O:1]1[C:12]2[C:4](=[CH:5][C:6](=[CH:10][CH:11]=2)[CH2:7][CH:8]=[CH2:9])[O:3][CH2:2]1.ClC1C=CC=C(C(OO)=[O:21])C=1.ClC1C=C(C=CC=1)C(O)=O>C(Cl)(Cl)Cl>[O:1]1[C:12]2[C:4](=[CH:5][C:6](=[CH:10][CH:11]=2)[CH2:7][CH:8]2[O:21][CH2:9]2)[O:3][CH2:2]1

参加物

5

反応物 3

HCID 4473-Chlorobenzoic AcidHCID 5144SafroleHCID 70297m-Chloroperbenzoic acid

生成物 1

HCID 101123Safrole oxide収率 39.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

16.2 g of safrole was dissolved in 100 ml of chloroform and to the mixture was added dropwise 20.7 g of m-chloroperbenzoic acid dissolved in 500 ml of chloroform at 0°-5° C. The resulting mixture was allowed to stand with slow stirring for 55 hours, while maintaining the temperature at 0° - 5° C. After the completion of the reaction, m-chlorobenzoic acid crystals were filtered and the filtrate was washed twice with 5% sodium hydroxide solution, and then with water. After drying over anhydrous sodium sulfate, the solvent was evaporated to obtain the residue. This was distilled under reduced pressure to give 7.0 g (yield 39.3%) of safrole oxide as colourless oily substance having a boiling point of 108° - 110° C/3 mmHg.

後処理

  1. temperaturewhile maintaining the temperature at 0° - 5° C
  2. filtrationwere filtered
  3. washthe filtrate was washed twice with 5% sodium hydroxide solution
  4. dry with materialAfter drying over anhydrous sodium sulfate
  5. customthe solvent was evaporated
  6. customto obtain the residue
  7. distillationThis was distilled under reduced pressure

出典と根拠

ORDレコード
ord-2b54d2f2b524405692cee26bdb19a316
出典データセット
uspto-grants-1977_12
特許番号
US04062862

関連ノート

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