Triethylamine → 5-Tert-butyl-2-methoxy-3-nitro-benzyl methanesulphonate
Reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[C:6]([C:10]1[CH:11]=[C:12]([N+:20]([O-:22])=[O:21])[C:13]([O:18][CH3:19])=[C:14]([CH2:16][OH:17])[CH:15]=1)([CH3:9])([CH3:8])[CH3:7].C(N(CC)CC)C>ClCCl>[CH3:1][S:2]([O:17][CH2:16][C:14]1[CH:15]=[C:10]([C:6]([CH3:9])([CH3:7])[CH3:8])[CH:11]=[C:12]([N+:20]([O-:22])=[O:21])[C:13]=1[O:18][CH3:19])(=[O:4])=[O:3]Participants
5
Procedure
1.20 ml methanesulphonic acid chloride are added to an ice-cooled solution of 3.43 g (5-tert-butyl-2-methoxy-3-nitro-phenyl)-methanol and 2.40 ml triethylamine in 30 ml dichloromethane. The solution is stirred for 2 h while cooling with ice and then diluted with dichloromethane. The dilute solution is washed three times with water and once with saturated aqueous saline solution, dried (MgSO4) and evaporated to dryness.
Workup
- temperaturewhile cooling with ice
- washThe dilute solution is washed three times with water
- dry with materialonce with saturated aqueous saline solution, dried (MgSO4)
- customevaporated to dryness
Sources & evidence
- ORD record
- ord-ebb7ea27afc8440e9b295b67aa1ca71a
- Source dataset
- uspto-grants-2015_02
- Patent number
- US08946438B2
Reaction notes
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