Sodium hydrosulfide hydrate → HCID 66702027, compound

HRID 424683Notes

Reaction equation

HRID 424683 reaction equation
O.[SH-].[Na+:3].C([S:11]([C:14]1[N:19]=[C:18]([N:20]([CH2:30][O:31][CH2:32][CH2:33][Si:34]([CH3:37])([CH3:36])[CH3:35])[S:21]([N:24]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)(=[O:23])=[O:22])[CH:17]=[C:16]([NH:38][C@H:39]([CH3:42])[CH2:40][OH:41])[N:15]=1)(=O)=O)C1C=CC=CC=1>CS(C)=O>[OH:41][CH2:40][C@H:39]([NH:38][C:16]1[CH:17]=[C:18]([N:20]([S:21]([N:24]2[CH2:25][CH2:26][O:27][CH2:28][CH2:29]2)(=[O:22])=[O:23])[CH2:30][O:31][CH2:32][CH2:33][Si:34]([CH3:37])([CH3:36])[CH3:35])[N:19]=[C:14]([S-:11])[N:15]=1)[CH3:42].[Na+:3]

Participants

4

Reactant 2

HCID 16211346Sodium hydrosulfide hydrate4×HCID 66701974HCID 66701974, compound

Product 1

HCID 66702027HCID 66702027, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent3×

Procedure

Sodium hydrosulfide hydrate (0.62 g) was added to a solution of the subtitle product of step iii) (2.5 g) in DMSO (5 ml) and the green solution stirred for 1.25 h. A further aliquot of sodium hydrosulfide hydrate (0.28 g) was added and stirred for 45 min. A further aliquot of sodium hydrosulfide hydrate (0.32 g) was added and stirred for 1.25 h before the addition of a final aliquot of sodium hydrosulfide hydrate (0.10 g) in DMSO (1 ml). The resulting reaction solution was diluted with DMSO (10 ml) and 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 107-110.

Workup

  1. stirringstirred for 45 min
  2. customThe resulting reaction solution

Sources & evidence

ORD record
ord-2f5df4c00a334057bc34f0e1e3400220
Source dataset
uspto-grants-2012_01
Patent number
US08106063B2

Reaction notes

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