تفاعل #160194

معادلة التفاعل

triethylamine

(4-isopropoxy-3-methyl-phenyl)-(8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)methanone

iodomethane

DCM

→

(4-isopropoxy-3-methyl-phenyl)-(10-methyl-8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)methanone hydrochloride salt

المردود 54.0%

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated in vacuo
2. 2
   workup.ADDITIONdiluted with methanol
3. 3
   ترشيحfiltered
4. 4
   أخرىpurified by prep LCMS (1-99% ACN/H2O, 5 mM HCl modifier)

الإجراء التجريبي

To (4-isopropoxy-3-methyl-phenyl)-(8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)methanone (22 mg, 0.05 mmol) in DCM (0.3 mL) was added iodomethane (15 mg, 7 μL, 0.11 mmol) followed by the addition of triethylamine (15 μL, 0.11 mmol) and the reaction mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated in vacuo, diluted with methanol, filtered and purified by prep LCMS (1-99% ACN/H2O, 5 mM HCl modifier) to give (4-isopropoxy-3-methyl-phenyl)-(10-methyl-8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)methanone hydrochloride salt as a glassy solid (13 mg, 54%). ESI-MS m/z calc. 422.3. Found 423.5 (M+1)+; Retention time: 1.31 minutes (3 min run).

المصدر