Dichloromethane → HCID 58424948, compound
Reaction equation
ClCCl.Cl.Cl.[O:6]1[CH2:11][CH2:10][N:9]([CH2:12][C:13]2[CH:14]=[CH:15][C:16]3[C:25]4[NH:24][CH2:23][CH2:22][CH2:21][C:20]=4[C:19](=[O:26])[NH:18][C:17]=3[CH:27]=2)[CH2:8][CH2:7]1.C(N(CC)CC)C>CO>[O:6]1[CH2:7][CH2:8][N:9]([CH2:12][C:13]2[CH:14]=[CH:15][C:16]3[C:25]4[NH:24][CH2:23][CH2:22][CH2:21][C:20]=4[C:19](=[O:26])[NH:18][C:17]=3[CH:27]=2)[CH2:10][CH2:11]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Dichloromethane (60 ml) and methanol (60 ml) were added to 8-(morpholinomethyl)-1,2,3,4-tetrahydrobenzo[h][1,6]naphthyridine-5(6H)-one dihydrochloride (13 g, 31.2 mmol) prepared in Example 49, and then triehylamine (13.05 ml, 93.6 mmol) was added dropwise at room temperature. After stirring at room temperature for 30 minutes, the precipitate was collected by filteration, washed with ethyl acetate (20 ml), and dried in vacuo to obtain the title compound (10 g, yield: 93%, white solid).
Workup
- customthe precipitate was collected by filteration
- washwashed with ethyl acetate (20 ml)
- customdried in vacuo
Sources & evidence
- ORD record
- ord-4e44540dc8dc4c928754c27b91a22a2c
- Source dataset
- uspto-grants-2014_08
- Patent number
- US08815891B2
Reaction notes
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