Sodium Hydroxide → 2-Nitro-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocycloheptene-4-carboxylic Acid Methyl Ester
Reaction equation
[CH3:1][O:2][C:3]([C:5]1[C:15]2[O:14][CH2:13][CH2:12][CH2:11][N:10](C=O)[C:9]=2[CH:8]=[C:7]([N+:18]([O-:20])=[O:19])[CH:6]=1)=[O:4].[N+]([NH-])([O-])=O.[OH-].[Na+]>Cl>[CH3:1][O:2][C:3]([C:5]1[C:15]2[O:14][CH2:13][CH2:12][CH2:11][NH:10][C:9]=2[CH:8]=[C:7]([N+:18]([O-:20])=[O:19])[CH:6]=1)=[O:4]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 100 °C
Procedure
The previously prepared nitroamide 9-formyl-2-nitro-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocycloheptene-4-carboxylic acid methyl ester (4.76 grams, 17 mmol) was suspended in 1N HCl and heated to 100° C. for 2 hours. After cooling to room temperature, the pH of the reaction mixture was adjusted to 12 with 1N NaOH. The precipitate formed was extracted with ethyl acetate. The latter was dried over anhydrous magnesium sulfate, filtered and evaporated.
Workup
- temperatureAfter cooling to room temperature
- customThe precipitate formed
- extractionwas extracted with ethyl acetate
- dry with materialThe latter was dried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated
Sources & evidence
- ORD record
- ord-d9118a11fea341b8b9e88bd724f167e5
- Source dataset
- uspto-grants-2004_11
- Patent number
- US06821977B2
Reaction notes
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