Sodium hydrosulfide hydrate → HCID 66702031, compound

HRID 729671Notes

Reaction equation

HRID 729671 reaction equation
O.[SH-].[Na+:3].C([S:11]([C:14]1[N:19]=[C:18]([N:20]([CH2:28][O:29][CH2:30][CH2:31][Si:32]([CH3:35])([CH3:34])[CH3:33])[S:21]([N:24]2[CH2:27][CH2:26][CH2:25]2)(=[O:23])=[O:22])[CH:17]=[C:16]([NH:36][C@H:37]([CH3:40])[CH2:38][OH:39])[N:15]=1)(=O)=O)C1C=CC=CC=1>CS(C)=O>[N:24]1([S:21]([N:20]([CH2:28][O:29][CH2:30][CH2:31][Si:32]([CH3:33])([CH3:35])[CH3:34])[C:18]2[CH:17]=[C:16]([NH:36][C@H:37]([CH3:40])[CH2:38][OH:39])[N:15]=[C:14]([S-:11])[N:19]=2)(=[O:22])=[O:23])[CH2:27][CH2:26][CH2:25]1.[Na+:3]

Participants

4

Reactant 2

HCID 16211346Sodium hydrosulfide hydrate2×HCID 66701995HCID 66701995, compound

Product 1

HCID 66702031HCID 66702031, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Conditions

Temperature
50 °C

Procedure

Sodium hydrosulfide hydrate (1.18 g) was added to a solution of the subtitle product of step iv) (8.0 g) in DMSO (67 ml) and the green solution stirred for 2 h. A farther aliquot of sodium hydrosulfide hydrate (0.79 g) was added and stirred for 1 h. This aliquot addition was repeated twice more before heating the solution at 50° C. for 30 min. The resulting reaction solution was used directly in the following step. The subtitle compound was also kept as a stock solution for further reaction with alkyl halides, described in Examples 41-42.

Workup

  1. stirringstirred for 1 h
  2. additionThis aliquot addition
  3. customThe resulting reaction solution

Sources & evidence

ORD record
ord-0e42bdcdba8445c79bb3b93075c93212
Source dataset
uspto-grants-2009_09
Patent number
US07582644B2

Reaction notes

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