Hydrochloric Acid → HCID 66755460, compound

HRID 1642977Notes

Reaction equation

HRID 1642977 reaction equation
[ClH:1].C(OC(=O)[NH:8][C:9]1([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)[CH2:12][CH2:11][CH2:10]1)(C)(C)C>O1CCOCC1>[ClH:1].[NH2:8][C:9]1([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:32])([F:31])[F:33])=[CH:26][CH:25]=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][CH2:11][CH2:10]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 58002137HCID 58002137, compound

Product 1

HCID 66755460HCID 66755460, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.4 ml (1.7 mmol) of a 4N solution of hydrogen chloride in dioxane was added to a solution of 100 mg (0.17 mmol) of the compound from Example 166 in 0.25 ml of dioxane. The reaction mixture was stirred at room temperature for 20 h. The mixture was concentrated under reduced pressure, again taken up in 0.25 ml of dioxane, and once more 0.4 ml (1.7 mmol) of a 4N solution of hydrogen chloride in dioxane was added. The reaction mixture was stirred at room temperature for 16 h. The mixture was then concentrated to dryness under reduced pressure and dried until the weight remained constant. Yield: 92 mg (100% of theory).

Workup

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additiononce more 0.4 ml (1.7 mmol) of a 4N solution of hydrogen chloride in dioxane was added
  3. stirringThe reaction mixture was stirred at room temperature for 16 h
  4. concentrationThe mixture was then concentrated to dryness under reduced pressure
  5. customdried until the weight

Sources & evidence

ORD record
ord-1496cf3c55cd4d939affca5183ded2bf
Source dataset
uspto-grants-2012_02
Patent number
US08119663B2

Reaction notes

Loading…