Acetone → HCID 178429849, compound
Reaction equation
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][C:3]=1[NH2:18].S(=O)(=O)(O)O.C(=O)([O-])[O-].[K+].[K+].[CH3:30][C:31]([CH3:33])=O>>[CH3:30][C:31]1([CH3:33])[NH:1][C:2]2[C:15]3[C:14](=[O:16])[C:13]4[C:8]([C:7](=[O:17])[C:6]=3[CH:5]=[CH:4][C:3]=2[NH:18]1)=[CH:9][CH:10]=[CH:11][CH:12]=4Participants
5
Procedure
1,2-Diaminoanthraquinone (1.19 g, 5 mmol) is dissolved in dry acetone (100 mL), and concentrated sulfuric acid (0.1 mL) is further added thereinto. After mixing and reacting in room temperature for 48 hours, the reacted mixture is transferred into a potassium carbonate column. The product is collected and recrystallized by methanol, so as to obtain the purple compound 20, and the production rate is 31%. In the purification steps of the Embodiment 21, regular extraction method will reduce the production rate, and thus the basic column is used to remove the acid in the rough extract, so as to increase the production rate.
Workup
- additionAfter mixing
- customThe product is collected
- customrecrystallized by methanol
Sources & evidence
- ORD record
- ord-f8802ee4af1c4905a5c6154d14b4e6da
- Source dataset
- uspto-grants-2013_05
- Patent number
- US08445492B2
Reaction notes
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