HCID 54369478, compound → HCID 54171837, compound

HRID 1248006Notes

Reaction equation

HRID 1248006 reaction equation
C([O:3][CH2:4][CH2:5][O:6][C:7]([N:9]1[CH2:14][CH2:13][CH2:12][S:11][C:10]1=[CH:15][N+:16]([O-:18])=[O:17])=[O:8])=O>ClCCl.CO>[OH:3][CH2:4][CH2:5][O:6][C:7]([N:9]1[CH2:14][CH2:13][CH2:12][S:11][C:10]1=[CH:15][N+:16]([O-:18])=[O:17])=[O:8]

Participants

3

Reactant 1

HCID 54369478HCID 54369478, compound

Product 1

HCID 54171837HCID 54171837, compoundYield 61.2%

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Procedure

The compound of Example 3 (2 g) was passed down a column of neutral alumina (200 g) using a dichloro methane/methanol mixture (95/5, v/v) as eluent at a flow rate of approximately 35 ml per minute. The eluted material was concentrated and purified by column chromatography on silica to afford the title compound (1.1 g) and recovered starting material (600 g). Melting point of the product was 59°-62° C.

Workup

  1. concentrationThe eluted material was concentrated
  2. custompurified by column chromatography on silica

Sources & evidence

ORD record
ord-341b0caac764428c964997c3e00c242f
Source dataset
uspto-grants-1985_06
Patent number
US04521536

Reaction notes

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