Water → HCID 12683887, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[C:17]3[NH:16][CH:15]=[N:14][C:13]=3[C:12](=[S:18])[N:11]3[CH2:19][CH2:20][N:21]=[C:10]23)=[CH:4][CH:3]=1.O.[OH-].[Na+].[CH3:25]I>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[C:17]3[C:13]([N:14]=[CH:15][N:16]=3)=[C:12]([S:18][CH3:25])[N:11]3[CH2:19][CH2:20][N:21]=[C:10]23)=[CH:4][CH:3]=1Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
The product of Procedure 75, 6.65 g. (0.021 mole), was dissolved in a mixture of 100 ml. of water and 15 ml. of ethanol containing 1.0 g. (0.025 mole) of sodium hydroxide. Methyl iodide, 7.09 g. (0.05 mole) was then added whereupon a precipitate commenced to form and developed into a thick slurry within 3 hrs. The solid was collected, air dried, and recrystallized from DMF with charcoal treatment, m.p. 254.0°-256.0° dec.
Workup
- dissolution(0.021 mole), was dissolved in a mixture of 100 ml
- addition(0.05 mole) was then added whereupon a precipitate
- customto form
- customThe solid was collected
- customair dried
- customrecrystallized from DMF with charcoal treatment, m.p. 254.0°-256.0° dec.
Sources & evidence
- ORD record
- ord-c1e94f5558f946608bee001c47f73fc8
- Source dataset
- uspto-grants-1987_02
- Patent number
- US04642345
Reaction notes
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