Sulfuric Acid → HCID 86590814, compound

HRID 1592957Notes

Reaction equation

HRID 1592957 reaction equation
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[F:6][C:7]([F:48])([F:47])[C:8]1[CH:9]=[C:10]([C@H:18]([N:20]([CH3:46])[C:21]([N:23]2[CH2:28][CH2:27][C@@H:26]([N:29]3[CH2:34][CH2:33][N:32]([C:35](=[O:37])[CH3:36])[CH2:31][CH2:30]3)[CH2:25][C@@H:24]2[C:38]2[CH:43]=[CH:42][C:41]([F:44])=[CH:40][C:39]=2[CH3:45])=[O:22])[CH3:19])[CH:11]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:13]=1>C1COCC1>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[F:17][C:14]([F:15])([F:16])[C:12]1[CH:11]=[C:10]([C@H:18]([N:20]([CH3:46])[C:21]([N:23]2[CH2:28][CH2:27][C@H:26]([N:29]3[CH2:30][CH2:31][N:32]([C:35](=[O:37])[CH3:36])[CH2:33][CH2:34]3)[CH2:25][C@@H:24]2[C:38]2[CH:43]=[CH:42][C:41]([F:44])=[CH:40][C:39]=2[CH3:45])=[O:22])[CH3:19])[CH:9]=[C:8]([C:7]([F:47])([F:6])[F:48])[CH:13]=1

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 51003178HCID 51003178, compound

Product 1

HCID 86590814HCID 86590814, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
23 °C

Procedure

Sulfuric acid 96% was added (0.06 mL) to a solution of example 1 b (0.65 g) in THF (6.5 mL) at 23° C. under a nitrogen atmosphere. The suspension was stirred at 23° C. for 15 hours, then cooled to 4° C., stirred for 4 hours and allowed to warm to r.t. The solid was filtered off and dried at 23° C. for 18 hours to give the title compound (0.681 g).

Workup

  1. temperaturecooled to 4° C.
  2. stirringstirred for 4 hours
  3. temperatureto warm to r.t
  4. filtrationThe solid was filtered off
  5. customdried at 23° C. for 18 hours

Sources & evidence

ORD record
ord-da784111911745d28a65bd7e24666179
Source dataset
uspto-grants-2007_11
Patent number
US07294630B2

Reaction notes

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