Hydrochloric Acid → HCID 13309002, compound
Reaction equation
[NH:1]1[CH2:6][CH2:5][O:4][CH:3]([CH:7]=[C:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH:12]=[CH:11][C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]2=3)[CH2:2]1.[CH2:23]=O.Cl>C(O)=O>[CH3:23][N:1]1[CH2:6][CH2:5][O:4][CH:3]([CH:7]=[C:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH:12]=[CH:11][C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]2=3)[CH2:2]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 5-(morpholin-2-yl)methylidene-5H-dibenzo[a,d]cycloheptene (0.35 g), 90% formic acid (0.7 g) and 37% formalin (0.65 ml) was stirred at 95° - 100° C for 6.5 hours. After cooling, 4N hydrochloric acid was added thereto, and the resulting mixture was evaporated to dryness under reduced pressure, neutralized with ammonia water and extracted with benzene. The benzene extract was washed with water, dried over anhydrous sodium sulfate and evaporated to afford 5-(4-methylmorpholin-2-yl)methylidene-5H-dibenzo-[a,d]cycloheptene as oily material. M.P., 237° - 238° C (decomp.) (oxalate).
Workup
- temperatureAfter cooling
- customthe resulting mixture was evaporated to dryness under reduced pressure
- extractionextracted with benzene
- extractionThe benzene extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- customevaporated
Sources & evidence
- ORD record
- ord-083f5cf8e8d543cba491cf9345817596
- Source dataset
- uspto-grants-1978_04
- Patent number
- US04085210
Reaction notes
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