HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 21471820, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Oxalate | HCID 71081 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 21471929 | HCID 21471929 | — |
| Product | HCID 21471820 | HCID 21471820 | — |
Reaction Steps
To a solution of 0.4 g of 3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)acetyl)-2-methyl-5,6,7,8-tetrahydro-4H-thieno[3,2-c]azepin-4-one (m.p. 175°-176° C. as oxalate thereof) in 20 ml of methanol was added 0.5 g of sodium borohydride under cooling. The mixture was stirred for 10 minutes and concentrated. Water was added thereto and the solution was extracted with ethyl acetate. The extract was washed with water, dried and the solvent was distilled away. The residue was treated with fumaric acid in ethanol and recrystallized from ethanol to give 0.22 g of 3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)-1-hydroxyethyl)-2-methyl-5,6,7,8-tetrahydro-4H-thieno[3,2-c]azepin-4-one difumarate monohydrate, m.p. 116°-118° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05532240 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-e643df3ba6804efcbcf6be23733c6c80 |
| Source note | uspto-grants-1996_07 |