Hydrochloric Acid → HCID 20230722, compound
Reaction equation
B.C1COCC1.[CH3:7][O:8][C:9]1[CH:23]=[CH:22][C:12]2[CH:13]3[CH:17]([CH2:18][CH2:19][C:11]=2[CH:10]=1)[C:16](=O)[NH:15][C:14]3=O.[ClH:24]>>[ClH:24].[CH3:7][O:8][C:9]1[CH:23]=[CH:22][C:12]2[CH:13]3[CH:17]([CH2:18][CH2:19][C:11]=2[CH:10]=1)[CH2:16][NH:15][CH2:14]3Participants
4
Procedure
BH3.THF (1M solution, 52 mL) was added to the compound of example 20 (1.5 g, 6.5 mmole). The reaction mixture was stirred at reflux for 2 hrs., cooled to 0°, and 10 mL 6N HCl added. After 2 hours reflux, solvents were evaporated. CH3CN was added and evaporated several times. The residue was crystallized from MeOH/Et2O to obtain 1.0 g white solid; M+ 203.
Workup
- temperatureat reflux for 2 hrs
- temperature, cooled to 0°
- temperatureAfter 2 hours reflux
- customsolvents were evaporated
- additionCH3CN was added
- customevaporated several times
- customThe residue was crystallized from MeOH/Et2O
Sources & evidence
- ORD record
- ord-d4f17fff4190430d944b6dd5c2c1fa24
- Source dataset
- uspto-grants-1986_10
- Patent number
- US04618683
Reaction notes
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