HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 178481557, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 178501105 | HCID 178501105 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 178481557 | HCID 178481557 | 85.1% |
Reaction Steps
LiOH (0.77 mmol, 0.02 g) was added to a solution of trans-4-(1-Methyl-2,5-dioxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepin-4-ylmethyl)-cyclohexane carboxylic acid methyl ester (0.64 mmol, 0.22 g) in 1:1 dioxane/water (16 mL) at 0° C. After 1 h at 0° C. the ice bath was removed and the mixture was allowed to reach room temperature. The reaction mixture was washed with DCM (1×20 mL). To the aqueous layer HCl 2N was added until acid pH, then extract with DCM (3×15 mL). The organic layer was washed with brine dried over Na2SO4 anhydrous and the solvent was removed under reduced pressure to obtain the titled compound (0.18 g, yield 85%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08865704B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-332a0537dce64d7e882c74662dea0ba7 |
| Source note | uspto-grants-2014_10 |