Sulfuric Acid → HCID 66636688, compound

HRID 44297Notes

Reaction equation

HRID 44297 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]1

Participants

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

  1. temperaturemaintaining the temperature between 60 and 70° C
  2. customis brought to ambient temperature
  3. waitAfter 30 minutes
  4. customthe red solid formed
  5. filtrationis filtered off
  6. washwashed intensively with ice-cold water
  7. dry with materialit is then dried in vacuo in the presence of P2O5 and at 40° C. overnight

Sources & evidence

ORD record
ord-5296c5fb6c684f62a1f52dd25ec74e71
Source dataset
uspto-grants-2013_09
Patent number
US08541412B2

Reaction notes

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