Chloride → HCID 178445943, compound

HRID 237347Notes

Reaction equation

HRID 237347 reaction equation
I.[OH:2][CH:3]1[C@@H:7]([NH:8][C:9](=[O:32])[C@H:10]([CH2:28][CH:29]([CH3:31])[CH3:30])[NH:11][C:12](=[NH:27])[C:13]2[CH:26]=[CH:25][C:24]3[S:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[NH:16][C:15]=3[CH:14]=2)[CH2:6][CH2:5][O:4]1.[Cl-:33]>O>[ClH:33].[OH:2][CH:3]1[C@@H:7]([NH:8][C:9](=[O:32])[C@H:10]([CH2:28][CH:29]([CH3:30])[CH3:31])[NH:11][C:12](=[NH:27])[C:13]2[CH:26]=[CH:25][C:24]3[S:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[NH:16][C:15]=3[CH:14]=2)[CH2:6][CH2:5][O:4]1

Participants

4

Reactant 2

HCID 312ChlorideHCID 178445944HCID 178445944, compound

Product 1

HCID 178445943HCID 178445943, compoundYield 74%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 2.5 g (4.4 mmoles) of the compound of Example 5 in 1 liter of distilled water is deposited at the top of a column containing approximately 10 equivalents of a Dowex-1×2 exchange resin previously equilibrated in the chloride form. The compound is eluted dropwise from the column using distilled water. The fractions containing the expected compound are collected and lyophilized. 1.55 g (yield: 74%) of a yellow solid is obtained. Melting point: 202-205° C.

Workup

  1. additioncontaining approximately 10 equivalents of a Dowex-1×2 exchange resin
  2. washThe compound is eluted dropwise from the column
  3. distillationusing distilled water
  4. additionThe fractions containing the expected compound
  5. customare collected

Sources & evidence

ORD record
ord-3ce196ad95844474baa877b33bd7b788
Source dataset
uspto-grants-2014_02
Patent number
US08642591B2

Reaction notes

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