HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → 3-[2-(N-t-butoxycarbonylglycyl)hydrazino]-5-methyl-6-phenyl-1,2,4-triazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | N-(tert-butoxycarbonyl)glycine | HCID 78288 | — |
| Reactant | 3-Hydrazino-5-methyl-6-phenyl-1,2,4-triazine | HCID 15586409 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-[2-(N-t-butoxycarbonylglycyl)hydrazino]-5-methyl-6-phenyl-1,2,4-triazine | HCID 20232077 | 75.8% |
Reaction Steps
The reaction of ethyl chloroformate (2.441 g) with N-t-butoxycarbonylglycine (3.938 g) in methylene chloride under ice cooling gave a solution comprising the mixed acid anhydride, which was reacted with 3-hydrazino-5-methyl-6-phenyl-1,2,4-triazine (3.015 g) in a similar manner to that of Example 17-(1) to give 3-[2-(N-t-butoxycarbonylglycyl)hydrazino]-5-methyl-6-phenyl-1,2,4-triazine (4.068 g). The purification was conducted with column chromatography on silica gel (80 g) using a mixture of methylene chloride and methanol (30:1) as an eluent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04616014 |
| Source dataset | uspto-grants-1986_10 |
| ORD ID | ord-7ab2032db55548c48dce9b4e15b59520 |
| Source note | uspto-grants-1986_10 |