Dichloromethane → HCID 57970970, compound
Reaction equation
Cl[C:2]([O:4][CH3:5])=[O:3].[NH:6]1[CH2:11][CH2:10][CH:9]([N:12]2[CH2:16][CH2:15][C:14]3([CH2:21][CH2:20][CH2:19][N:18]([C:22]4[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][N:23]=4)[CH2:17]3)[C:13]2=[O:32])[CH2:8][CH2:7]1.C(N(CC)C(C)C)(C)C.C(Cl)Cl>>[O:32]=[C:13]1[C:14]2([CH2:21][CH2:20][CH2:19][N:18]([C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:30])([F:31])[F:29])=[CH:24][N:23]=3)[CH2:17]2)[CH2:15][CH2:16][N:12]1[CH:9]1[CH2:10][CH2:11][N:6]([C:2]([O:4][CH3:5])=[O:3])[CH2:7][CH2:8]1Participants
5
Procedure
Methyl chloroformate (4.4 μL, 0.000057 mol) was added to a solution of 2-piperidin-4-yl-7-[5-(trifluoromethyl)pyridin-2-yl]-2,7-diazaspiro[4.5]decan-1-one (18.3 mg, 0.0000478 mol) and N,N-diisopropylethylamine (27 μL, 0.00016 mol) in methylene chloride (1.0 mL, 0.016 mol); and the mixture was stirred for 0.5 h. The volatiles were removed in-vacuo and the product was purified by prep-HPLC. LC-MS: 441.2 (M+H)+.
Workup
- customThe volatiles were removed in-vacuo
- customthe product was purified by prep-HPLC
Sources & evidence
- ORD record
- ord-f2b2d9b268ac475ca374b12f4a8a5b95
- Source dataset
- uspto-grants-2012_02
- Patent number
- US08110581B2
Reaction notes
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