Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-Boc-1-methylhydrazine | HCID 3748280 | 92.2% |
Reaction Steps
Di-tert-butyl-dicarbonate (0.23.69 g, 108.5 mmol) in methanol (40 mL) was added dropwise over a period of 1.5 h to a solution of methylhydrazine (5.00 g, 106.4 mmol) in methanol (20 mL) cooled to ˜5° C. When the addition was complete, tlc (10% methanol/dichloromethane) indicated that the reaction was complete. The reaction mixture was stored at −20° C. overnight, and then the solvent was evaporated to give N-methyl-hydrazinecarboxylic acid tert-butyl ester (14.34 g, 92%) as a colorless oil which was used directly in the subsequent step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07622492B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-3dbcc68fa70945deb12f7059960ed119 |
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| Source note | uspto-grants-2009_11 |
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