Sulfuric Acid → HCID 21556755, 화합물

HRID 267290노트

반응식

HRID 267290 반응식
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

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 21556733HCID 21556733, 화합물

생성물 1

HCID 21556755HCID 21556755, 화합물수율 80.4%

시약·촉매·용매 1

HCID 23994Zinc촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1ebf4483d0454bc588225bf5b6e85b63
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941826

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