Methylenechloride Hexane → HCID 22005193, compound
Reaction equation
[CH:1]([C:4]1[C:5]([CH2:22][O:23][CH2:24][C:25]2[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=2)=[C:6]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:7]([CH2:13][OH:14])=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:3])[CH3:2].[CH2:32](Cl)Cl.CCCCCC>>[CH:1]([C:4]1[C:5]([CH2:22][O:23][CH2:24][C:25]2[CH:26]=[CH:27][C:28]([CH3:31])=[CH:29][CH:30]=2)=[C:6]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:7]([CH:13]([OH:14])[CH3:32])=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:2])[CH3:3]Participants
3
Procedure
The title compound was prepared by subjecting the intermediate obtained in Step A to the procedures described in Example 244, Steps I-K. mp 84-86° C.; Rf=0.1 (80% CH2Cl2/hexane); 1H NMR (300 MHz, CDCl3): δ 7.39 (s, 1H), 7.27 (m, 2H), 7.09 (m, 6H), 4.76 (dq, J=1.5, 7 Hz, 1H), 4.22 (s, 2H), 4.03 (s, 2H), 3.89 (septet, J=6.6 Hz, 1H), 3.26 (septet, J=6.6 Hz, 1H), 2.35 (s, 3H), 1.66 (s, 1H), 1.40 (d, J=6.6 Hz, 3H), 1.26 (m, 12H); FAB-MS calcd for (C29H35FO2) 434, found 417 (M—OH); Anal. Calcd for C29H35FO2: C, 80.15; H, 8.12; F, 4.37. Found: C, 80.10; H, 8.30; F, 4.24; [α]22=+30.7.
Sources & evidence
- ORD record
- ord-4f08d4b1fd4a4962a37c5346b159422d
- Source dataset
- uspto-grants-2001_04
- Patent number
- US06218431B1
Reaction notes
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