HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methylbenzenesulfonic acid → HCID 24755527, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| Reactant | Triethyl orthoacetate | HCID 66221 | — |
| Reactant | HCID 15055101 | HCID 15055101 | — |
| Product | HCID 24755527 | HCID 24755527 | — |
Reaction Steps
3-(3-Hydroxy-2,2-dimethyl-propylamino)-2,2-dimethyl-propan-1-ol (128.0 g, 0.68 mol), triethyl orthoacetate (162.0 g, 1.00 mol) and toluene sulfonic acid (2.0 g) were charged into a oven dried round bottom flask equipped with a stirring bar, distillation head and under nitrogen. The resulting solution was heated until the theoretical amount of methanol was collected. The reaction was cooled to room temperature and triethylamine added to neutralize the acid. Fractional vacuum distillations (twice) afforded the product as a water clear liquid, boiling point 101-103° C. at 0.44 torr. Yield: 156 g (90.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07812173B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-9e6414aa04ca42a6a0001cc174cc7262 |
| Source note | uspto-grants-2010_10 |