2-Methylbenzenesulfonic acid → 2-Chloromethyl-4,4,6,6-tetramethyl-1,3-dithiane

HRID 127141

반응식

HRID 127141 반응식
[Cl:1][CH2:2][CH:3](OC)OC.[CH3:8][C:9]([SH:16])([CH2:11][C:12]([CH3:15])([SH:14])[CH3:13])[CH3:10].C1(C)C(S(O)(=O)=O)=CC=CC=1>>[Cl:1][CH2:2][CH:3]1[S:16][C:9]([CH3:10])([CH3:8])[CH2:11][C:12]([CH3:15])([CH3:13])[S:14]1

참가 물질

4

반응물 3

HCID 69252-Methylbenzenesulfonic acidHCID 609862-Chloro-1,1-dimethoxyethaneHCID 202861032,4-Dimethyl-2,4-pentanedithiol

생성물 1

HCID 202861232-Chloromethyl-4,4,6,6-tetramethyl-1,3-dithiane

실험 절차

2-Chloro-1,1-dimethoxyethane (0.1 mole) and 2,4-dimethyl-2,4-pentanedithiol (0.1 mole) are charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, Dean Stark trap and reflux condenser. Toluene sulfonic acid (0.1 grams) is added and the reaction mixture is heated and thiol removed. When the thiol evolution ceases, the reaction mixture is then cooled to room temperature, treated with sodium carbonate (5 grams) and filtered. Volatiles are stripped from the filtrate using a rotary evaporator to yield the desired product 2-chloromethyl-4,4,6,6-tetramethyl-1,3-dithiane as the residue.

후처리

  1. customfitted with a mechanical stirrer
  2. temperaturethermometer, Dean Stark trap and reflux condenser
  3. temperaturethe reaction mixture is heated
  4. customthiol removed
  5. additiontreated with sodium carbonate (5 grams)
  6. filtrationfiltered
  7. customa rotary evaporator

출처 및 근거

ORD 기록
ord-1cebef1484be4b479df47b97bc4f2cf4
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255182

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