Hydrochloric Acid → HCID 67000243, compound

HRID 560176Notes

Reaction equation

HRID 560176 reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[F:27])[CH:19]=2)[NH:14][C:13]=1[C:28]([OH:30])=[O:29])=O)(C)(C)C.[ClH:31].C(OCC)C>C(Cl)Cl.O1CCOCC1>[ClH:31].[NH2:8][CH2:9][CH2:10][CH2:11][C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[F:27])[CH:19]=2)[NH:14][C:13]=1[C:28]([OH:30])=[O:29]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 58172109HCID 58172109, compound

Product 1

HCID 67000243HCID 67000243, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 312751,4-DioxaneSolvent

Procedure

To the above carboxylic acid (13 mg, 0.031 mmol, 1.0 equiv) in methylene chloride (2 mL) at 0° C. was added 0.2 mL of 4 N HCl in dioxane. The reaction was stirred at ambient temperature for 1 h. Then 10 mL of diethyl ether was added to the reaction and the reaction concentrated. To this residue was added 5 mL diethyl ether and the solid was filtered off and washed with diethyl ether several times and air dried for 15 min to provide the title compound (8 mg); MS, electrospray, 313 (M+H).

Workup

  1. concentrationthe reaction concentrated
  2. additionTo this residue was added 5 mL diethyl ether
  3. filtrationthe solid was filtered off
  4. washwashed with diethyl ether several times and air
  5. customdried for 15 min

Sources & evidence

ORD record
ord-cb39e838f70249db9e60cea77c0b4bcc
Source dataset
uspto-grants-2011_11
Patent number
US08063094B2

Reaction notes

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