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

HRID 127141

反応式

HRID 127141 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1cebef1484be4b479df47b97bc4f2cf4
出典データセット
uspto-grants-1981_03
特許番号
US04255182

関連ノート

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