1,4-Dioxane hydrochloride → HCID 68421313, compound
Reaction equation
[ClH:1].O1CCOCC1.[CH:8]1[C:18]2[CH:17]=[CH:16][C:15]3[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=3[C:13](=[C:23]3[CH2:28][CH2:27][N:26]([C:29](=[O:45])[CH2:30][CH2:31][N:32]([CH2:40][C:41]([CH3:44])([CH3:43])[CH3:42])C(=O)OC(C)(C)C)[CH2:25][CH2:24]3)[C:12]=2[CH:11]=[CH:10][CH:9]=1>>[ClH:1].[CH:19]1[C:15]2[CH:16]=[CH:17][C:18]3[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=3[C:13](=[C:23]3[CH2:24][CH2:25][N:26]([C:29](=[O:45])[CH2:30][CH2:31][NH:32][CH2:40][C:41]([CH3:43])([CH3:42])[CH3:44])[CH2:27][CH2:28]3)[C:14]=2[CH:22]=[CH:21][CH:20]=1Participants
3
Procedure
5 ml of 4 N hydrochloric acid/1,4-dioxane solution was added to 184.1 mg (0.357 mmol) of t-butyl 3-[4-(5H-dibenzo[a,d][7]annulen-5-ylidene)-1-piperidinyl]-3-oxopropyl(neopentyl)carbamate, and they were stirred for 1 hour. The solvent was evaporated under reduced pressure. 5 ml of diethyl ether was added to the residue, and then 1 ml of 4 N hydrochloric acid/ethyl acetate solution was added thereto. The precipitates thus formed were taken by the filtration, washed with diethyl ether and dried under reduced pressure to obtain the title compound.
Workup
- customThe solvent was evaporated under reduced pressure
- addition5 ml of diethyl ether was added to the residue
- addition1 ml of 4 N hydrochloric acid/ethyl acetate solution was added
- customThe precipitates thus
- customformed
- filtrationwere taken by the filtration
- washwashed with diethyl ether
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-c0de98e1cdb942f69f984c3fbc764e16
- Source dataset
- uspto-grants-2008_12
- Patent number
- US07462630B2
Reaction notes
Loading…