Sulfuric Acid → HCID 21556755、化合物

HRID 267290ノート

反応式

HRID 267290 の反応式
S(=O)(=O)(O)O.[Br:6][C:7]1[C:12]([CH:13]([CH2:15][CH3:16])[CH3:14])=[CH:11][C:10]([S:17](Cl)(=O)=O)=[C:9]([CH:21]([CH2:23][CH3:24])[CH3:22])[CH:8]=1>[Zn]>[Br:6][C:7]1[C:12]([CH:13]([CH2:15][CH3:16])[CH3:14])=[CH:11][C:10]([SH:17])=[C:9]([CH:21]([CH2:23][CH3:24])[CH3:22])[CH:8]=1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 21556733HCID 21556733、化合物

生成物 1

HCID 21556755HCID 21556755、化合物収率 80.4%

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

実験手順

A 128-ml portion of concentrated sulfuric acid was added to 300 g of ice while keeping the temperature at 0°-10°C. Then 41 g of 4-bromo-2,5-di-sec-butylbenzenesulfonyl chloride was added. While maintaining the temperature at 0°-10°C, 65 g of zinc dust was added with good agitation over a period of 2 hours. The reaction mixture was then heated under reflux on a steam bath for 5 hours. After cooling, the mixture was extracted into methylene dichloride, dried over magnesium sulfate, filtered, and concentrated to an oil which was distilled, to give 27 g of 4-bromo-2,5-di-sec-butylbenzenethiol, bp 106°-107°C/0.22 mm, nD25 1.5599.

後処理

  1. customat 0°-10°C
  2. temperatureWhile maintaining the temperature at 0°-10°C
  3. temperatureThe reaction mixture was then heated
  4. temperatureunder reflux on a steam bath for 5 hours
  5. temperatureAfter cooling
  6. extractionthe mixture was extracted into methylene dichloride
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to an oil which
  10. distillationwas distilled

出典と根拠

ORDレコード
ord-1ebf4483d0454bc588225bf5b6e85b63
出典データセット
uspto-grants-1976_03
特許番号
US03941826

反応ノート

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