Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Dibenzo-p-dioxin | HCID 9216 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Product | HCID 87133463 | HCID 87133463 | — |
Reaction Steps
Dibenzo[b,e][1,4]dioxine (2 g, 10.86 mmol), was taken in dichloromethane (10 ml), 2-chloroacetyl chloride (2.0 ml, 24.97 mmol) was added and the reaction was cooled to −78° C. Aluminium chloride (5.79 g, 43.4 mmol) was added carefully and was stirred for additional 2 h at −78° C., then slowly allowed to reach rt and stirred for additional 2 h. Cooled to 0° C. and ice was added, stirred for few min, white precipitation noticed, MeOH (5 mL) was added and stirred for 1 h. The precipitate was filtered and washed with water and used in the next step. Yield: 1.8, 50%; ES LC-MS m/z=337 (M−H+);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08889726B2 |
|---|
| Source dataset | uspto-grants-2014_11 |
|---|
| ORD ID | ord-d72030cbda484be3b20627f0064077b6 |
|---|
| Source note | uspto-grants-2014_11 |
|---|