HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66782272, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 66782011 | HCID 66782011 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66782272 | HCID 66782272 | — |
Reaction Steps
A solution of 60.0 mmol of (1-amino-5-methoxyindan-1-yl)methanol in 120 ml of acetonitrile and 40 ml of methanol is cooled to −10° C. and 69 mmol of triethylamine and, dropwise over the course of 1 hour, 80.5 mmol of chloroacetyl chloride are successively added. The reaction mixture is warmed to room temperature and stirred for 3 hours. The reaction mixture is poured into water and extracted with tert-butyl methyl ether. The combined organic phases are washed with brine, dried with sodium sulphate and evaporated. The title compound is obtained as a beige solid which is employed without further purification for the next stage. Rf=0.15 (ethyl acetate-heptane 1:1); Rt=3.01 (gradient I).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08138179B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-2b38ccbc58e843bbbbbbe91054e3230a |
| Source note | uspto-grants-2012_03 |