Hydrochloric Acid → HCID 66755474, compound

HRID 1643122Notes

Reaction equation

HRID 1643122 reaction equation
[ClH:1].C(OC([N:9]1[CH2:12][CH:11]([C:13]2[O:17][N:16]=[C:15]([CH:18]3[CH2:23][CH:22]([C:24]4[CH:29]=[CH:28][C:27]([C:30]([F:33])([F:32])[F:31])=[CH:26][CH:25]=4)[CH2:21][N:20]([C:34]([N:36]4[CH2:41][CH2:40][O:39][CH2:38][CH2:37]4)=[O:35])[CH2:19]3)[N:14]=2)[CH2:10]1)=O)(C)(C)C>O1CCOCC1>[ClH:1].[NH:9]1[CH2:10][CH:11]([C:13]2[O:17][N:16]=[C:15]([CH:18]3[CH2:23][CH:22]([C:24]4[CH:25]=[CH:26][C:27]([C:30]([F:32])([F:33])[F:31])=[CH:28][CH:29]=4)[CH2:21][N:20]([C:34]([N:36]4[CH2:37][CH2:38][O:39][CH2:40][CH2:41]4)=[O:35])[CH2:19]3)[N:14]=2)[CH2:12]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 58002123HCID 58002123, compound

Product 1

HCID 66755474HCID 66755474, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.30 ml (1.16 mmol) of a 4N solution of hydrogen chloride in dioxane was added to a solution of 67 mg (0.117 mmol) of the compound from Example 92A in 0.6 ml of dioxane. The reaction mixture was stirred at room temperature for 20 hours. The mixture was concentrated using a rotary evaporator and once more taken up in 0.6 ml of dioxane, and 0.3 ml (1.16 mmol) of a 4N solution of hydrogen chloride in dioxane was added. The reaction mixture was stirred at room temperature overnight and then concentrated to dryness under reduced pressure and dried until the weight remained constant. Yield: 58 mg (100% of theory).

Workup

  1. concentrationThe mixture was concentrated
  2. customa rotary evaporator
  3. addition0.3 ml (1.16 mmol) of a 4N solution of hydrogen chloride in dioxane was added
  4. stirringThe reaction mixture was stirred at room temperature overnight
  5. concentrationconcentrated to dryness under reduced pressure
  6. customdried until the weight

Sources & evidence

ORD record
ord-bf200607533e449680a6c13d10ed9af6
Source dataset
uspto-grants-2012_02
Patent number
US08119663B2

Reaction notes

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