Dichloromethane → HCID 86662056, compound

HRID 869257Notes

Reaction equation

HRID 869257 reaction equation
[CH3:1][N:2]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)[CH2:3][CH2:4][OH:5].ClCCl.C(N(CC)CC)C.[S:25](Cl)([CH3:28])(=[O:27])=[O:26]>O>[CH3:28][S:25]([O:5][CH2:4][CH2:3][N:2]([CH3:1])[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)(=[O:27])=[O:26]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 20538799HCID 20538799, compound

Product 1

HCID 86662056HCID 86662056, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a mixture of 2-[methyl(3-nitrophenyl)amino]ethanol (780 mg) and dichloromethane (20 mL), triethylamine (0.66 mL) and mesyl chloride (0.37 mL) were added sequentially under ice cooling and stirred for 3 hours. Water was added to the reaction liquid, and the organic layer was separated and washed with saturated aqueous sodium chloride. After drying over anhydrous magnesium sulfate, the solvent was distilled off to give 2-[methyl(3-nitrophenyl)amino]ethyl methanesulfonate (1.0 g) as a yellow solid.

Workup

  1. additionwere added sequentially under ice cooling
  2. customthe organic layer was separated
  3. washwashed with saturated aqueous sodium chloride
  4. dry with materialAfter drying over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off

Sources & evidence

ORD record
ord-769d024997d94a58bd8085dcbd652ddb
Source dataset
uspto-grants-2015_03
Patent number
US08969336B2

Reaction notes

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