Dichloromethane → HCID 67832220, compound

HRID 728773Notes

Reaction equation

HRID 728773 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[C:6]1([OH:17])(O)[CH:15]2[CH:10]([CH2:11]CCC2)[CH2:9][CH2:8][CH2:7]1.C(N([CH2:23][CH3:24])CC)C.Cl[CH2:26]Cl>>[CH3:1][S:2]([CH:24]1[CH2:23][CH2:11][CH:10]2[CH:9]([CH2:8][CH2:7][CH:6]([OH:17])[CH2:15]2)[CH2:26]1)(=[O:4])=[O:3]

Participants

5

Reactant 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 21710999HCID 21710999, compound

Product 1

HCID 67832220HCID 67832220, compound

Procedure

25.5 g (0.22 mole) of methanesulfonyl chloride were added dropwise, at 0°-5° C., to an initially taken mixture of 34 g (0.2 mole) of decalindiol and 30.3 g (0.3 mole) of triethylamine in 500 ml of dichloromethane. Stirring was then carried out for a further hour at room temperature. The mixture was poured onto ice, the organic phase was separated off and the aqueous phase was extracted several times with dichloromethane. The combined organic phases were washed with dilute hydrochloric acid, water and 5% strength sodium bicarbonate solution, dried over sodium sulfate and evaporated down under reduced pressure.

Workup

  1. waitwas then carried out for a further hour at room temperature
  2. additionThe mixture was poured onto ice
  3. customthe organic phase was separated off
  4. extractionthe aqueous phase was extracted several times with dichloromethane
  5. washThe combined organic phases were washed with dilute hydrochloric acid, water and 5% strength sodium bicarbonate solution
  6. dry with materialdried over sodium sulfate
  7. customevaporated down under reduced pressure

Sources & evidence

ORD record
ord-0dc93833f5c14fcc99d12e765b38d6f8
Source dataset
uspto-grants-1991_09
Patent number
US05051409

Reaction notes

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