HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → 5-Benzyloxy-6-methoxy-2H-phthalazin-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 3-benzyloxy-N,N-diethyl-2-formyl-4-methoxy-benzamide | HCID 18504788 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 5-Benzyloxy-6-methoxy-2H-phthalazin-1-one | HCID 18374642 | 96% |
Reaction Steps
Glacial acetic acid (285 ml) at 10-20° C. was dropwise added with hydrazine monohydrate (10.16 ml, 209 mmoles) and added with 3-benzyloxy-N,N-diethyl-2-formyl-4-methoxy-benzamide (14.27 g, 41.8 mmoles), prepared as described in example 56. The mixture was left to stand for 2 hours, then evaporated, dissolved in CH2Cl2, washed with water, anhydrified over Na2SO4, brought to dryness, and the crude was triturated in petrolatum/ethyl ether 2:1 (150 ml) and filtered to give 11.3 g of the title compound (yield: 96%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329370B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-796d27652c63437a918f70eaff8f2295 |
| Source note | uspto-grants-2001_12 |