Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 14013289 | HCID 14013289 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 14013068 | HCID 14013068 | 72% |
Reaction Steps
A mixture of 4 parts of 2-amino-N-[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl)methyl]-1-piperidinyl]ethyl]benzamide, 20 parts of acetic acid anhydride and 40 parts of water was stirred and heated overnight at 120° C. After cooling, ice water was added. The whole was treated with ammonium hydroxide. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was converted into the (E)-2-butenedioate salt in ethanol. The salt was filtered off and dried, yielding 3.7 parts (72%) of 3-[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]methyl]-1-piperidinyl]ethyl]-2-methyl-4(3H)-quinazolinone (E)-2-butenedioate (1:1); mp. 210.3° C. (481).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04839374 |
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| Source dataset | uspto-grants-1989_06 |
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| ORD ID | ord-ef8398e55e2646d7849509357bf737b3 |
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| Source note | uspto-grants-1989_06 |
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