HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Tert-butyl 3-(methanesulfonyloxy)azetidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Tert-butyl 3-hydroxyazetidine-1-carboxylate | HCID 2756801 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | Tert-butyl 3-(methanesulfonyloxy)azetidine-1-carboxylate | HCID 10753243 | 94% |
Reaction Steps
To 3-hydroxy-azetidine-1-carboxylic acid tert-butyl ester (1.21 g, 6.99 mmol) and Et3N (0.85 g, 1.2 mL, 8.4 mmol) in CH2Cl2 (35 mL) at 0° C. was added methanesulfonyl chloride (0.88 g, 0.60 mL, 7.7 mmol). After 1 h, brine was added and the reaction extracted with CH2Cl2 (2×). The combined organics were dried to give 1.65 g (94%) of 3-methanesulfonyloxy-azetidine-1-carboxylic acid tert-butyl ester a yellow solid that was used without further purification. 1H NMR (CDCl3): 5.20 (tt, J=6.7, 4.2 Hz, 1H), 4.28 (ddd, J=10.3, 6.7, 1.2 Hz, 2H), 4.10 (ddd, J=10.4, 4.2, 1.1 Hz, 2H), 3.07 (s, 3H), 1.44 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575364B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-9dcd449d82f047049f32d59044e05c12 |
| Source note | uspto-grants-2013_11 |