Methanesulfonic Acid → HCID 13760254, compound

HRID 893324Notes

Reaction equation

HRID 893324 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][C:19]=1[O:20][CH3:21])[CH2:6][NH:7][CH2:8][CH:9](O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CS(O)(=O)=O>ClCCl>[CH3:21][O:20][C:19]1[CH:18]=[C:17]2[C:5](=[CH:4][C:3]=1[O:2][CH3:1])[CH2:6][NH:7][CH2:8][CH:9]2[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 4719987T6668830

Product 1

HCID 13760254HCID 13760254, compoundYield 421.9%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Add the amino-alcohol from step A (2.2 g) to a mixture of methanesulfonic acid (100 mL) and dichloromethane (150 mL) and stir overnight at room temperature. Pour the mixture into ice-water, separate and concentrate the organic layer to a residue. Triturate with benzene then recrystallize from ethanol to give 8.7 g of the title amine as the methanesulfonate salt, mp=198°-199° C.

Workup

  1. customseparate
  2. concentrationconcentrate the organic layer to a residue
  3. customTriturate with benzene
  4. customthen recrystallize from ethanol

Sources & evidence

ORD record
ord-b31db5b93fa64d7694624aa086bdacb7
Source dataset
uspto-grants-1992_06
Patent number
US05124337

Reaction notes

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