Sulfuric Acid → 1,3-DITHIANE-2-CARBONYL CHLORIDE

HRID 268323

반응식

HRID 268323 반응식
OS(O)(=O)=O.[S:6]1[CH2:11][CH2:10][CH2:9][S:8][CH:7]1[C:12]([OH:14])=O.C(Cl)(=O)C([Cl:18])=O>C1C=CC=CC=1>[S:6]1[CH2:11][CH2:10][CH2:9][S:8][CH:7]1[C:12]([Cl:18])=[O:14]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 65578Oxalyl chlorideHCID 3037051,3-Dithiane-2-carboxylic acid

생성물 1

HCID 122220081,3-DITHIANE-2-CARBONYL CHLORIDE

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

In a 500 ml. reaction flask equipped with a reflux condenser connected with a wash-bottle containing H2SO4, there are added 250 ml. of anhydrous benzene (distilled upon sodium), 42 g (0.25 mol) of 1.3-dithiane-2-carboxylic acid (as prepared in example 1) and 28 ml. (0.4 mol) of freshly distilled oxalyl chloride. The mixture is stirred at room temperature and at the end of gaseous evolution, the mixture is heated up to 45° C to complete the gas evolution. The solvent and the excess of oxalyl chloride are evaporated under reduced pressure and the residue is crystallized from dried cyclohexane to yield 1.3-dithiane-2-carboxylic acid chloride.

후처리

  1. customreaction flask
  2. customequipped with a reflux condenser
  3. additionare added 250 ml
  4. temperaturethe mixture is heated up to 45° C
  5. customThe solvent and the excess of oxalyl chloride are evaporated under reduced pressure
  6. customthe residue is crystallized from dried cyclohexane

출처 및 근거

ORD 기록
ord-6495b24d022747268f8f4b0fcc14670a
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947469

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