HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19922086, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 86747457 | HCID 86747457 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 19922086 | HCID 19922086 | 77% |
Reaction Steps
To a mixture of 0.442 g (0.73 mmol) of 4-[6-[3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]hexyl]-3-(3-ethoxy-3-oxopropyl)-δ-oxobenzenepentanoic acid ethyl ester from the preceding example, in 7 mL of tetrahydrofuran and 7 mL of water was added 91.7 mg (2.19 mmol) of lithium hydroxide monohydrate and the reaction was stirred for room temperature for 19.3 hr. After being acidified with 16 mL of 3N aqueous sulfuric acid, the mixture was worked-up with ethyl acetate in the usual manner. The crude product thus obtained was recrystallized from hexane-ethyl acetate to give 0.309 g (77%) of the title compound as a white solid, mp 136°-139° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05273999 |
| Source dataset | uspto-grants-1993_12 |
| ORD ID | ord-4f6c296025914207873fb22206922a84 |
| Source note | uspto-grants-1993_12 |