Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Diazomethane | HCID 9550 | — |
| Reactant | HCID 69256115 | HCID 69256115 | — |
| Reactant | HCID 71352260 | HCID 71352260 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131726855 | HCID 131726855 | — |
Reaction Steps
4 (2.00 g, 4.76 mmol) was dissolved in 15 ml of dry THF and converted into a mixed anhydride (see compound 1) using CAIBE (0.623 ml, 4.76 mmol) and NMM (0.525 ml, 4.76 mmol). The precipitate formed was filtered off and cooled down to −15° C. Then diazomethane (23.8 mmol in 30 ml ether) was dropped into the solution under an argon atmosphere. After leaving the mixture for 1 h at 0° C. 1.27 ml of HBr (33% in AcOH) was added and the solution was stirred for 30 min at room temperature . . . . After that 70 ml of ether was added and the mixture was washed with 20 ml of water. The organic layer was separated and dried (Na2SO4) and evaporated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07368421B2 |
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| Source dataset | uspto-grants-2008_05 |
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| ORD ID | ord-0c68ad533f4948ffb19d755dfa8158df |
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| Source note | uspto-grants-2008_05 |
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