HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21563685, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Thiophosgene | HCID 10040 | — |
| Reactant | HCID 21563668 | HCID 21563668 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 21563685 | HCID 21563685 | 36.2% |
Reaction Steps
An amount of 35 g of thiophosgene, 250 ml of dioxane and 100 ml of water is placed into a sulphating flask and cooled to 0° to 5°; an addition is then made dropwise, within 30 minutes, of a solution of 61 g of 2-(3'-aminophenoxy)-1-methylbenzimidazole in 200 ml of dioxane. The mixture is stirred for 3 hours at 0° to 5°; it is afterwards further stirred for 15 hours at room temperature. After dilution with 600 ml of water, the precipitate is separated and stirred, for 7 hours at 10°, into a solution of 10 g of thiophosgene in 500 ml of acetone. The product is separated and recrystallized from acetonitrile to obtain 29.3 g of (3'-isothiocyanophenoxy)-1-methylbenzimidazolehydrochloride, M.P. 154° to 158°C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03933841 |
| Source dataset | uspto-grants-1976_01 |
| ORD ID | ord-992bbf66d6254d07ab106b9f68f6d3e8 |
| Source note | uspto-grants-1976_01 |