Phosphorus pentachloride → 3-Azidopropane-1-sulfonyl chloride

HRID 239709ノート

反応式

HRID 239709 の反応式
[N:1]([CH2:4][CH2:5][CH2:6][S:7]([OH:10])(=O)=[O:8])=[N+:2]=[N-:3].[Na].P(Cl)(Cl)(Cl)(Cl)[Cl:13]>C1C=CC=CC=1>[N:1]([CH2:4][CH2:5][CH2:6][S:7]([Cl:13])(=[O:10])=[O:8])=[N+:2]=[N-:3]

参加物

5

反応物 3

HCID 24819Phosphorus pentachlorideHCID 5360545SodiumHCID 589318663-Azidopropane-1-sulfonic acid

生成物 1

HCID 538209503-Azidopropane-1-sulfonyl chloride

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

3-Azidopropanesulfonic acid, sodium salt 5 (1.87 g, 10.0 mmol) was suspended in dry benzene (20 mL), and PCl5 (2.3 g, 10.5 mmol) was added to the suspension. The mixture was stirred at room temperature for 30 minutes, then at gentle reflux for about 1 hour. The benzene and P(O)Cl3 were removed by evaporation under reduced pressure. Benzene was added to the crude mixture and the solvent was removed again under reduced pressure. The residue was dried in vacuo. The dried residue was dissolved in dichloromethane (anhydrous, 15 mL) and cooled at −10° C. using an ice/acetone bath.

後処理

  1. temperatureat gentle reflux for about 1 hour
  2. customThe benzene and P(O)Cl3 were removed by evaporation under reduced pressure
  3. additionBenzene was added to the crude mixture
  4. customthe solvent was removed again under reduced pressure
  5. customThe residue was dried in vacuo
  6. dissolutionThe dried residue was dissolved in dichloromethane (anhydrous, 15 mL)
  7. temperaturecooled at −10° C.

出典と根拠

ORDレコード
ord-ddb9760233e0443a99dec0afc31a7ac8
出典データセット
uspto-grants-2014_02
特許番号
US08642801B2

反応ノート

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