Sulfuric Acid → 1,3-Dithiane-2-carbonyl chloride

HRID 268323

反応式

HRID 268323 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 122220081,3-Dithiane-2-carbonyl chloride

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6495b24d022747268f8f4b0fcc14670a
出典データセット
uspto-grants-1976_03
特許番号
US03947469

関連ノート

読み込み中…