Sodium hydrosulfide hydrate → HCID 66701922, compound
Reaction equation
O.[SH-].[Na+:3].C([S:11][C:12]1[N:17]=[C:16]([N:18]([CH2:27][O:28][CH2:29][CH2:30][Si:31]([CH3:34])([CH3:33])[CH3:32])[S:19]([N:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)(=[O:21])=[O:20])[CH:15]=[C:14]([NH:35][C@H:36]([CH3:39])[CH2:37][OH:38])[N:13]=1)C1C=CC=CC=1>CS(C)=O>[OH:38][CH2:37][C@H:36]([NH:35][C:14]1[CH:15]=[C:16]([N:18]([S:19]([N:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)(=[O:20])=[O:21])[CH2:27][O:28][CH2:29][CH2:30][Si:31]([CH3:33])([CH3:34])[CH3:32])[N:17]=[C:12]([S-:11])[N:13]=1)[CH3:39].[Na+:3]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Sodium hydrosulfide hydrate (2.15 g) was added to a solution of the subtitle product of step iii) (4.5 g) in DMSO (37.8 ml) and the green solution stirred for 1 h. A further aliquot of sodium hydrosulfide hydrate (0.1 g) was added and stirred for 1 h. A further aliquot of sodium hydrosulfide hydrate (0.1 g) was added and stirred for 2 h before the addition of a final aliquot of sodium hydrosulfide hydrate (0.05 g). 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 112-113.
Workup
- stirringstirred for 1 h
- customThe resulting reaction solution
Sources & evidence
- ORD record
- ord-7fd88065b26e4c96a4e9448e5fd4d415
- Source dataset
- uspto-grants-2009_09
- Patent number
- US07582644B2
Reaction notes
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