Hydrochloric Acid → HCID 66755542, compound

HRID 1642978Notes

Reaction equation

HRID 1642978 reaction equation
[ClH:1].C(OC(=O)[NH:8][C:9]1([C:12]2[O:16][N:15]=[C:14]([CH:17]3[CH2:22][CH:21]([C:23]4[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=4)[CH2:20][N:19]([C:33]([N:35]4[CH2:40][CH2:39][O:38][CH2:37][CH2:36]4)=[O:34])[CH2:18]3)[N:13]=2)[CH2:11][CH2:10]1)(C)(C)C>O1CCOCC1>[ClH:1].[NH2:8][C:9]1([C:12]2[O:16][N:15]=[C:14]([CH:17]3[CH2:22][CH:21]([C:23]4[CH:28]=[CH:27][C:26]([C:29]([F:31])([F:32])[F:30])=[CH:25][CH:24]=4)[CH2:20][N:19]([C:33]([N:35]4[CH2:40][CH2:39][O:38][CH2:37][CH2:36]4)=[O:34])[CH2:18]3)[N:13]=2)[CH2:11][CH2:10]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 58002426HCID 58002426, compound

Product 1

HCID 66755542HCID 66755542, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.6 ml (2.3 mmol) of a 4N solution of hydrogen chloride in dioxane was added to a solution of 130 mg (0.230 mmol) of the compound from Example 85A 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 0.6 ml (2.3 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: 115 mg (92% of theory).

Workup

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additiononce more 0.6 ml (2.3 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-f6aa0783a1914b1fa5c13fa9b6a8c7f4
Source dataset
uspto-grants-2012_02
Patent number
US08119663B2

Reaction notes

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