Methanesulfonyl chloride → HCID 20501226, compound

HRID 851446Notes

Reaction equation

HRID 851446 reaction equation
[CH3:1][C:2]1([CH3:18])[O:6][C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=2[Cl:16])([CH2:7][OH:8])[C:4](=[O:17])[O:3]1.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>N1C=CC=CC=1>[CH3:1][C:2]1([CH3:18])[O:6][C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=2[Cl:16])([CH2:7][O:8][S:20]([CH3:19])(=[O:22])=[O:21])[C:4](=[O:17])[O:3]1

Participants

4

Procedure

63.5 g (0.22 mole) of 2,2-dimethyl-4-(2,4-dichlorophenyl)-4-hydroxymethyl-1,3-dioxolan-5-one are dissolved in 400 ml of pyridine and to this solution are added 28.9 g of methanesulfonyl chloride at 0° to 5° C. The resultant suspension is stirred for 2 hours at the same temperature, then poured into ice-water and extracted with methylene chloride. The extract is washed with water, dried over sodium sulfate and evaporated to dryness. The residual resin is crystallised by addition of a small amount of diethyl ether/hexane and the product is isolated by filtration. Melting point: 98°-100° C.

Workup

  1. extractionextracted with methylene chloride
  2. washThe extract is washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness
  5. customThe residual resin is crystallised by addition of a small amount of diethyl ether/hexane
  6. customthe product is isolated by filtration

Sources & evidence

ORD record
ord-9fe68f965a5a4cbabf0cc445bee4a2e8
Source dataset
uspto-grants-1983_05
Patent number
US04384879

Reaction notes

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