1,4-Dioxane hydrochloride → HCID 178465286, compound
Reaction equation
C(OC(=O)[NH:7][CH:8]([C:10](=[O:23])[NH:11][C:12]1[NH:13][N:14]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:16]=1)[CH3:9])(C)(C)C.O1CCOCC1.[ClH:31]>>[ClH:31].[ClH:31].[NH2:7][CH:8]([CH3:9])[C:10]([NH:11][C:12]1[NH:13][N:14]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:16]=1)=[O:23]Participants
3
Procedure
To 100 mg (0.30 mmol) of the product of Step A [1-(5-phenyl-2H-pyrazol-3-ylcarbamoyl)-ethyl]-carbamic acid tert-butyl ester was added 1 ml of 4N HCl dioxane solution (Aldrich) at ambient temperature. The reaction was allowed to stir for 3 hours. After evaporation to dryness and trituration with ether, 73 mg of amino-N-(5-phenyl-2H-pyrazol-3-yl)-propionamide dihydrochloride was obtained as a white powder (80%) ( MS: 231[P+1]/229 [P−1])(RF=0.2 on silica TLC (9/1 Chloroform/ Methanol).
Workup
- customAfter evaporation to dryness and trituration with ether
Sources & evidence
- ORD record
- ord-49149d3a9c5243bc8c2cfc9d9f5da193
- Source dataset
- uspto-grants-2009_04
- Patent number
- US07521464B2
Reaction notes
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