Hydrochloric Acid → HCID 68554501, compound
Reaction equation
Cl.[CH2:2]([CH2:5][NH2:6])[CH:3]=[CH2:4].[O:7]1[C:11]2([CH2:16][CH2:15][C:14](=O)[CH2:13][CH2:12]2)[O:10][CH2:9][CH2:8]1.[C-:18]#[N:19].[K+]>CO.O>[CH2:2]([CH2:5][NH:6][C:14]1([C:18]#[N:19])[CH2:15][CH2:16][C:11]2([O:10][CH2:9][CH2:8][O:7]2)[CH2:12][CH2:13]1)[CH:3]=[CH2:4]Participants
7
Procedure
A mixture of 9 ml water, 5.3 ml hydrochloric acid (32 per cent by weight), 8 ml methanol, 17.5 g allylmethylamine, 8.00 g 1,4-dioxaspiro[4.5]decan-8-one and 8.0 g potassium cyanide was stirred for 65 hours at room temperature. The yellowish-white suspension obtained was extracted four times with 25 ml diethyl ether each time, the combined extracts were dried over sodium sulfate, filtered and concentrated and the residue was largely freed from solvent residues in vacuo. 11.3 g 8-(allylmethylamino)-1,4-dioxaspiro[4.5]decane-8-carbonitrile were obtained as a pale brown liquid.
Workup
- customThe yellowish-white suspension obtained
- extractionwas extracted four times with 25 ml diethyl ether each time
- dry with materialthe combined extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-a56641bc89c74891b7e4e61d9e1a4bda
- Source dataset
- uspto-grants-2010_03
- Patent number
- US07678834B2
Reaction notes
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