Hydroxybenzenesulfonic acid → HCID 86672603, compound

HRID 470688Notes

Reaction equation

HRID 470688 reaction equation
O.[C:2]1([S:8]([OH:11])(=[O:10])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12]([C@H:15]1[O:20][CH2:19][C@H:18]([NH:21][C:22]([C@@H:24]2[NH:38][C:37]3([CH2:43][CH2:42][C:41]([CH3:45])([CH3:44])[CH2:40][CH2:39]3)[C@:26]3([C:34]4[C:29](=[CH:30][C:31]([Cl:35])=[CH:32][CH:33]=4)[NH:28][C:27]3=[O:36])[C@H:25]2[C:46]2[CH:51]=[CH:50][N:49]=[C:48]([Cl:52])[C:47]=2[F:53])=[O:23])[CH2:17][CH2:16]1)(=[O:14])[NH2:13]>CC(O)C>[OH2:9].[C:2]1([S:8]([OH:11])(=[O:10])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12]([C@H:15]1[O:20][CH2:19][C@H:18]([NH:21][C:22]([C@@H:24]2[NH:38][C:37]3([CH2:39][CH2:40][C:41]([CH3:45])([CH3:44])[CH2:42][CH2:43]3)[C@:26]3([C:34]4[C:29](=[CH:30][C:31]([Cl:35])=[CH:32][CH:33]=4)[NH:28][C:27]3=[O:36])[C@H:25]2[C:46]2[CH:51]=[CH:50][N:49]=[C:48]([Cl:52])[C:47]=2[F:53])=[O:23])[CH2:17][CH2:16]1)(=[O:14])[NH2:13]

Participants

4

Reactant 2

HCID 15619088Hydroxybenzenesulfonic acidHCID 73297272Milademetan

Product 1

HCID 86672603HCID 86672603, compoundYield 171.7%

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

Benzenesulfonic acid monohydrate (30 mg, 0.17 mmol) was added to a 2-propanol (1.0 ml) solution of the compound (104 mg, 0.17 mmol) obtained in Example 70 and the resulting mixture was dissolved by heating. After stirring at room temperature for 24 hours, the precipitate was collected by filtration to give 116 mg (89%) of the title compound as a solid.

Workup

  1. dissolutionthe resulting mixture was dissolved
  2. temperatureby heating
  3. filtrationthe precipitate was collected by filtration

Sources & evidence

ORD record
ord-bd6c961b6f7141969ce7b8c2f5ddfd4c
Source dataset
uspto-grants-2014_01
Patent number
US08629133B2

Reaction notes

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