HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisobutylaluminum hydride → HCID 90014767, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 118119931 | HCID 118119931 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 90014767 | HCID 90014767 | 79% |
Reaction Steps
A mixture comprising 4.42 g (10.36 mmol) (RS)-ethyl 4-[(2-oxo-2,3-dihydro-1,3-benzothiazol-6-yl)amino]-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-7-carboxylate (prepared according to example 1) 350 mL tetrahydrofuran and 62.1 mL hydrido(diisobutyl)aluminum (1M in tetrahydrofuran) was stirred at 23° C. overnight. 40 mL saturated ammonium chloride was added carefully and stirring was continued for 0.5 hours. The precipitate was filtered off and washed with ethyl acetate. The product crystallized from the filtrate and was washed with water and a mixture of dichloromethane and methanol to give 3.13 g (79%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296757B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-c0bd9be012c1474e922b0dcbfbce3092 |
| Source note | uspto-grants-2016_03 |