Water → HCID 15713246, compound

HRID 847375Notes

Reaction equation

HRID 847375 reaction equation
[CH:1]([N:3]1[CH:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:7][C:6](=[CH2:14])[CH2:5][C:4]1(C(OCC)=O)[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[O:2].[Cl-].[Na+].O>CS(C)=O>[CH:1]([N:3]1[CH:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:7][C:6](=[CH2:14])[CH2:5][CH:4]1[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[O:2]

Participants

5

Reactant 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 15713245HCID 15713245, compound

Product 1

HCID 15713246HCID 15713246, compoundYield 101.4%

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Conditions

Temperature
165 °C

Procedure

A mixture of 5 g of the product of Step B, 0.8 g of sodium chloride, 0.26 g of water and 15 ml of dimethylsulfoxide was stirred for 3 hours at 165° C. and the mixture was returned to ambient temperature followed by filtering, washing and evaporating to dryness to obtain 4 g of product which was purified on silica eluting with a cyclohexane-ethyl acetate (9-1) mixture, then by a cyclohexane-ethyl acetate (7-3) mixture to obtain 3.1 g of the desired product with a Rf=0.5.

Workup

  1. customwas returned to ambient temperature
  2. filtrationby filtering
  3. washwashing
  4. customevaporating to dryness

Sources & evidence

ORD record
ord-bd0833d4b10847f09e1a2bffa53b4633
Source dataset
uspto-grants-1992_08
Patent number
US05141952

Reaction notes

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