Hydrazine hydrate (1:1) → HCID 62678395, compound
Reaction equation
O.[NH2:2][NH2:3].C([O:6][C:7](=O)[C:8]([CH3:12])([CH3:11])[CH2:9][CH3:10])C>>[CH3:11][C:8]([CH3:12])([CH2:9][CH3:10])[C:7]([NH:2][NH2:3])=[O:6]Participants
3
Procedure
Reflux a mixture of hydrazine monohydrate (0.97 g, 19.4 mmol) and 2,2-dimethyl-butyric acid ethyl ester (1.4 g, 9.7 mmol) for 72 hours. Purify the crude material by flash chromatography (silica gel) using 5% (7 M ammoniated methanol) in dichloromethane to afford the title compound (0.78 g). 1H NMR (CDCl3) δ 0.81 (t, 3H), 1.13 (s, 6H), 1.53 (q, 2H), 3.88 (s, 2H), 7.05 (bs, 1H).
Workup
- temperatureReflux
- customPurify the crude material by flash chromatography (silica gel)
Sources & evidence
- ORD record
- ord-48c2c415982b4132b4270e2108bcc8a0
- Source dataset
- uspto-grants-2013_11
- Patent number
- US08592590B2
Reaction notes
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