Methanesulfonic Acid → HCID 22748383, compound
Reaction equation
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH2:13][CH3:14])=[CH:4][C:3]=1[C:15]([NH:17][CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]([CH2:31][CH3:32])([CH3:30])[CH3:29])=[CH:24][C:23]=1[C:33]([CH2:36][CH3:37])([CH3:35])[CH3:34])=[O:16].[N+:38]([C:41]1[CH:50]=[CH:49][C:44]([O:45]CCO)=[CH:43][CH:42]=1)([O-:40])=[O:39].CS(O)(=O)=O>>[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH2:13][CH2:14][O:45][C:44]2[CH:49]=[CH:50][C:41]([N+:38]([O-:40])=[O:39])=[CH:42][CH:43]=2)=[CH:4][C:3]=1[C:15]([NH:17][CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]([CH2:31][CH3:32])([CH3:30])[CH3:29])=[CH:24][C:23]=1[C:33]([CH2:36][CH3:37])([CH3:34])[CH3:35])=[O:16]Participants
4
Procedure
By heating a mixture of 5 g of Intermediate 2, 12 g of β-(4-nitrophenoxy)ethanol, and 0.3 g of methanesulfonic acid to 140-150° C for 3 hours under a reduced pressure, the desired product was obtained. The solvent used for the recrystallization of the product was acetonitrile. The melting point of the product was 166-168° C.
Workup
- temperatureBy heating
Sources & evidence
- ORD record
- ord-82665e3cd41a4c1fa2780197c61572cc
- Source dataset
- uspto-grants-1979_02
- Patent number
- US04138258
Reaction notes
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