Sulfuric Acid → HCID 66636688, compound
Reaction equation
ON=[CH:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][N:15]2[CH2:19][CH2:18][O:17][C:16]2=[O:20])=[CH:9][CH:8]=1)=[O:5].[OH:21]S(O)(=O)=O>>[O:20]=[C:16]1[N:15]([CH2:14][CH2:13][C:10]2[CH:11]=[C:12]3[C:7](=[CH:8][CH:9]=2)[NH:6][C:4](=[O:5])[C:3]3=[O:21])[CH2:19][CH2:18][O:17]1Participants
3
Conditions
- Temperature
- 80 °C
Procedure
Concentrated H2SO4 (20 ml) is heated to 50° C. The compound obtained in Step D (25.24 mmoles) is added slowly in solid form, maintaining the temperature between 60 and 70° C. The reaction mixture is then stirred for one hour at 80° C. The mixture is brought to ambient temperature and then poured onto 200 g of crushed ice. After 30 minutes, the red solid formed is filtered off and washed intensively with ice-cold water; it is then dried in vacuo in the presence of P2O5 and at 40° C. overnight to yield the title product, which is used directly in the next Step.
Workup
- temperaturemaintaining the temperature between 60 and 70° C
- customis brought to ambient temperature
- waitAfter 30 minutes
- customthe red solid formed
- filtrationis filtered off
- washwashed intensively with ice-cold water
- dry with materialit is then dried in vacuo in the presence of P2O5 and at 40° C. overnight
Sources & evidence
- ORD record
- ord-b97ea827daf64c9b9a8e92732fcb737e
- Source dataset
- uspto-grants-2014_02
- Patent number
- US08653073B2
Reaction notes
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