Methanol → HCID 21534902, compound
Reaction equation
[CH:1]1([CH:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:17])[NH:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CO>C(Cl)(Cl)Cl>[CH:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:17])[NH:9][CH:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
50 g of 4-cyclohexyl-3,4-dihydro-2H-isoquinoline-1-one and 20 l g of methanol-wet 30% Pd/C were heated while to 220° C in a stream of argon. Thin-layer chromatographic analysis revealed that the reaction was practically completed after 75 minutes. The product was dissolved in chloroform, the catalyst was separated and the organic phase was evaporated. After recrystallization from acetone, colorless crystals were obtained. M.p. 111° to 112° C
Workup
- customthe catalyst was separated
- customthe organic phase was evaporated
- customAfter recrystallization from acetone
- customcolorless crystals were obtained
Sources & evidence
- ORD record
- ord-42d5da2834dc42539469445f7d68a375
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03961062
Reaction notes
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