HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 10262941, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | HCID 10398026 | HCID 10398026 | — |
| Reactant | HCID 10997193 | HCID 10997193 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10262941 | HCID 10262941 | — |
| Product | 1,3-Dihydro-1-methyl-2H-pyrrolo[2,3-b]pyridine-2-thione | HCID 10329636 | — |
Reaction Steps
P2S5 (3.80 g, 8.10 mmol) was added to a vigorously stirred suspension of Na2CO3 (0.88 g, 8.10 mmol) in THF (30 mL). After the mixture had become homogeneous (ca. 15 minutes), a solution of 1-methyl-7-aza-2-indolinone [VII: R1 =7-aza, R3 =Me] (1.00 g) in THF (10 mL) was added and stirring was continued for 18 hours at 20° C. Solvent was removed under reduced pressure, and the residue was partitioned between EtOAc and water. Workup of the organic layer, and chromatography of the residue on silica gel (elution with EtOAc/petroleum ether (1:5)) gave 1-methyl-7-aza-2-indolinethione [IX: R1 =7-aza, R3 =Me] (0.81 g, 73%); mp (EtOAc/petroleum ether) 130°-133° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05464861 |
| Source dataset | uspto-grants-1995_11 |
| ORD ID | ord-4238a882f22a4de9be45767f60db083a |
| Source note | uspto-grants-1995_11 |