Thionyl Chloride → HCID 19972458, compound
Reaction equation
S(Cl)([Cl:3])=O.O[CH2:6][CH2:7][N:8]([CH3:29])[C:9]([C:11]1[C:20]2[O:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[C:17]([CH3:27])[C:16](=[O:28])[C:15]=2[CH:14]=[CH:13][CH:12]=1)=[O:10]>ClCCl.C(OCC)C>[CH3:29][N:8]([CH2:7][CH2:6][Cl:3])[C:9]([C:11]1[C:20]2[O:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[C:17]([CH3:27])[C:16](=[O:28])[C:15]=2[CH:14]=[CH:13][CH:12]=1)=[O:10]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
A solution of 1.1 ml of thionyl chloride in 2 ml of dichloromethane was added to a solution of 3.37 g of Intermediate XIII in 20 ml of dichloromethane, and the mixture was stirred for 4 hours at ambient temperature. Removal of the solvent gave an oil which was taken up in diethyl ether. The title compound precipitated as a white solid which was filtered off for use without further purification. m.p. (118) 126°-128° C. (diethyl ether).
Workup
- customRemoval of the solvent
- customgave an oil which
- customThe title compound precipitated as a white solid which
- filtrationwas filtered off for use without further purification
- customm.p. (118) 126°-128° C. (diethyl ether)
Sources & evidence
- ORD record
- ord-af2845b701de4280964cff0ba515baef
- Source dataset
- uspto-grants-1997_02
- Patent number
- US05605896
Reaction notes
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