Methanol → HCID 69142839, compound
Reaction equation
[F:1][C:2]([F:28])([F:27])[O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]2)=[O:11])=[CH:6][CH:5]=1.CO.[ClH:31].CCOCC>>[ClH:31].[F:28][C:2]([F:1])([F:27])[O:3][C:4]1[CH:26]=[CH:25][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]2)=[O:11])=[CH:6][CH:5]=1Participants
4
Procedure
A solution of 174 mg (0.49 mmol) piperazine-1,4-dicarboxylic acid tert-butyl ester 4-trifluoromethoxy-benzyl ester in 4.9 ml 1.5M HCl/Et2O and 0.98 ml abs. MeOH was stirred at rt for 3 h. Evaporation of the reaction mixture provided 189 mg as colourless powder. 1H-NMR (d6-DMSO): 3.10 m, 4H and 3.62 m, 4H; 5.13 2, 2H; 7.40 d, 2H and 7.53 d, 2H, AB-system; 9.2 br, 2H. MS (ISP): 305.2 (M+H)+.
Workup
- customEvaporation of the reaction mixture
- customprovided 189 mg as colourless powder
- custom7.40 d, 2H and 7.53 d, 2H, AB-system
Sources & evidence
- ORD record
- ord-dc2a9b080f50485a93704c623f300238
- Source dataset
- uspto-grants-2006_04
- Patent number
- US07022707B2
Reaction notes
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