Dichloromethane → HCID 53410796, compound
Reaction equation
FC(F)(F)C(O)=O.C(O[C:13](=O)[N:14]([CH2:16][C:17](=[O:22])[NH:18][CH2:19][CH:20]=[CH2:21])C)(C)(C)C.C(Cl)[Cl:25]>>[ClH:25].[CH2:19]([NH:18][C:17](=[O:22])[CH2:16][NH:14][CH3:13])[CH:20]=[CH2:21]Participants
4
Procedure
Trifluoroacetic acid (7 ml) was added to a solution of the resulting allylcarbamoylmethyl-methyl-carbamic acid tert-butyl ester in methylene chloride (14 ml), and the mixture was stirred at room temperature for three hours. The reaction solution was concentrated under reduced pressure, and 4 N hydrochloric acid-dioxane was then added to the resulting residue. The mixture was concentrated under reduced pressure again to give N-allyl-2-methylamino-acetamide hydrochloride (577 mg). This was used in the next reaction without complete purification.
Workup
- concentrationThe reaction solution was concentrated under reduced pressure, and 4 N hydrochloric acid-dioxane
- additionwas then added to the resulting residue
- concentrationThe mixture was concentrated under reduced pressure again
Sources & evidence
- ORD record
- ord-18860938b98a4cceb9f7b4919da32f19
- Source dataset
- uspto-grants-2015_10
- Patent number
- US09169254B2
Reaction notes
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