Dichloromethane → HCID 70617081, compound

HRID 259078Notes

Reaction equation

HRID 259078 reaction equation
Cl[CH2:2]Cl.[CH3:4][C:5]([O:7][CH2:8][C:9]1[CH2:28][S:27][C@@H:12]2[C@H:13]([NH:16][C:17]([C@H:19]([NH2:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:18])[C:14](=[O:15])[N:11]2[C:10]=1[C:29]([OH:31])=[O:30])=[O:6].O.S([O-])([O-])(=O)=O.[Mg+2]>C(N(CC)CC)C>[CH3:4][C:5]([O:7][CH2:8][C:9]1[CH2:28][S:27][C@@H:12]2[C@H:13]([NH:16][C:17]([C@H:19]([NH2:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:18])[C:14](=[O:15])[N:11]2[C:10]=1[C:29]([OH:31])=[O:30])=[O:6].[CH2:14]([N:11]([CH2:10][CH3:29])[CH2:12][CH3:2])[CH3:13]

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 7061048122202-75-1

Product 1

HCID 70617081HCID 70617081, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

In 100 ml. of dichloromethane was suspended 4.25 g. of cephaloglycin monohydrate and then 2.8 ml. of triethylamine was dissolved therein. Furthermore, 5 g. of anhydrous magnesium sulphate was added to the system and after stirring the mixture for about 10 minutes at room temperature, the mixture was filtered to provide a solution of cephaloglycin triethylamine salt. The solution was cooled to -20° C. and the suspension of 4-hydroxynicotinoyl chloride prepared above was added dropwise to the solution with stirring. Thereafter, the cooling bath was removed to raise the temperature up to room temperature and the mixture was stirred for about one hour at room temperature.

Workup

  1. filtrationthe mixture was filtered

Sources & evidence

ORD record
ord-be03905c4dff4dd1a25cf4a2635f5bf0
Source dataset
uspto-grants-1977_07
Patent number
US04036834

Reaction notes

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