Sodium Hydroxide → HCID 14550002, compound
Reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([CH2:11][S:12][CH2:13][CH2:14][OH:15])[CH:5]=1)([O-])=O.[OH-].[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+]>O>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([CH2:11][S:12][CH2:13][CH2:14][OH:15])[CH:5]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
0.085 moles (19.5 g) of 4-nitro-2-[(β-hydroxyethylthio)methyl]phenol are added to a solution of 16 g of sodium hydroxide (NaOH) pellets in 135 ml of water, followed portionwise, so as to maintain the temperature between 70° C. and 75° C., by 55 g of sodium hydrosulphite. After the end of addition stirring is continued for 20 minutes at 75° C. After cooling, the expected product is precipitated by neutralizing the reaction mixture with acetic acid. After filtering off, followed by washing with water and drying, the product obtained is recrystallized from acetonitrile. It melts at 121° C.
Workup
- temperatureso as to maintain the temperature between 70° C. and 75° C.
- additionAfter the end of addition
- temperatureAfter cooling
- customthe expected product is precipitated
- filtrationAfter filtering off
- washby washing with water
- customdrying
- customthe product obtained
- customis recrystallized from acetonitrile
Sources & evidence
- ORD record
- ord-8312f326eee8430fa7280d193ade6b7f
- Source dataset
- uspto-grants-1991_10
- Patent number
- US05053052
Reaction notes
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