Hydrochloric Acid → HCID 57780675, compound
Reaction equation
Cl.[OH:2][C:3]([CH3:8])([CH3:7])[CH2:4][C:5]#[N:6].[CH2:9]([O:11]CC)[CH3:10]>>[CH2:9]([O:11][C:5](=[NH:6])[CH2:4][C:3]([OH:2])([CH3:8])[CH3:7])[CH3:10]Participants
4
Procedure
HCl (g) was bubbled through a solution of 3-hydroxy-3-methylbutyronitrile (5.0 g, 50.4 mmol) in diethyl ether (20 mL) and IMS (3.48 g, 75.6 mmol) at 0° C. for 30 minutes before leaving to stand at −5° C. over night. The solution was concentrated under vacuum affording 6.48 g (72%) of 3-hydroxy-3-methyl-butyrimidic acid ethyl ester. 1H NMR (400 MHz, CDCl3) δ: 11.36 (m br, 1H), 4.66 (q, 2H), 2.89 (s, 2H), 1.51 (t, 3H), 1.36 (s, 6H).
Workup
- custombefore leaving
- waitto stand at −5° C. over night
- concentrationThe solution was concentrated under vacuum
Sources & evidence
- ORD record
- ord-f26c1d7e23444039a7c21631560952c5
- Source dataset
- uspto-grants-2013_06
- Patent number
- US08461328B2
Reaction notes
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