Benzene → HCID 54240701, compound
Reaction equation
[CH2:1]1[O:14][C:13]2[C:3](=[CH:4][C:5]3[CH2:11][CH2:10][NH:9][CH2:8][CH2:7][C:6]=3[CH:12]=2)[O:2]1.C1C=CC=CC=1.[OH-].[Na+].[Cl:23][CH2:24][C:25](Cl)=[O:26]>O>[Cl:23][CH2:24][C:25]([N:9]1[CH2:10][CH2:11][C:5]2[CH:4]=[C:3]3[O:2][CH2:1][O:14][C:13]3=[CH:12][C:6]=2[CH2:7][CH2:8]1)=[O:26]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
One-tenth mole, 22.7 g, of 2,3,4,5-tetrahydro-7,8-methylenedioxy-1H-3-benzazepine was dissolved in 200 ml of water and 200 ml of benzene added. Forty ml of a 10% solution of sodium hydroxide was added to the vigorously stirred emulsion and 17 g (0.15 mole) of chloroacetyl chloride was added dropwise. As the pH approached 5, another 10-ml portion of 10% sodium hydroxide solution was added until a total of 100 ml has been added. After all the chloroacetyl chloride had been added, the mixture, which has an acid reaction, was stirred for another 10 minutes then allowed to stand overnight at room temperature.
Workup
- additionwas added dropwise
- additionhas been added
- customan acid reaction
- waitto stand overnight at room temperature
Sources & evidence
- ORD record
- ord-37bd1aac4d654aab97facab07eb497f8
- Source dataset
- uspto-grants-1977_12
- Patent number
- US04065473
Reaction notes
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