Hydrochloric Acid → HCID 67456106, compound

HRID 242278Notes

Reaction equation

HRID 242278 reaction equation
[ClH:1].[N:2]1([C:8]2[N:13]=[CH:12][N:11]=[C:10]([N:14]3[C:18](=[O:19])[C:17]([N:20]4[CH:24]=[CH:23][N:22]=[N:21]4)=[CH:16][NH:15]3)[CH:9]=2)[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1>O1CCOCC1>[ClH:1].[N:2]1([C:8]2[N:13]=[CH:12][N:11]=[C:10]([N:14]3[C:18](=[O:19])[C:17]([N:20]4[CH:24]=[CH:23][N:22]=[N:21]4)=[CH:16][NH:15]3)[CH:9]=2)[CH2:3][CH2:4][O:5][CH2:6][CH2:7]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 59603622Molidustat

Product 1

HCID 67456106HCID 67456106, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

Batch 1: 7.5 ml of a 4 N solution of hydrogen chloride in dioxane are added to 1.7 g (5.4 mmol) of the compound from Example 71. The mixture is stirred at RT, 5 ml dioxane are added and the mixture is stirred at RT for 16 h. The solid is filtered off and washed with 5 ml dioxane. The mixture is dried under a high vacuum for 16 h, 10 ml methanol are then added and the mixture is stirred at RT for 1 h. The solid is filtered off, washed with 4 ml methanol and dried under a high vacuum. 1.6 g of the title compound are obtained.

Workup

  1. stirringthe mixture is stirred at RT for 16 h
  2. filtrationThe solid is filtered off
  3. washwashed with 5 ml dioxane
  4. customThe mixture is dried under a high vacuum for 16 h
  5. addition10 ml methanol are then added
  6. stirringthe mixture is stirred at RT for 1 h
  7. filtrationThe solid is filtered off
  8. washwashed with 4 ml methanol
  9. customdried under a high vacuum

Sources & evidence

ORD record
ord-c6186a386bee42548ec2a1ae4e624a27
Source dataset
uspto-grants-2014_02
Patent number
US08653111B2

Reaction notes

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