Methanesulfonic Acid → HCID 87756849, compound

HRID 1182049Notes

Reaction equation

HRID 1182049 reaction equation
Cl.CC(C)CCN[C:7]1[C:8]([C:23]([NH2:25])=[O:24])=[C:9]([CH3:22])[C:10]2[CH2:16][CH2:15][C:14]3[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=3[O:12][C:11]=2[CH:21]=1.[CH3:27][S:28]([OH:31])(=[O:30])=[O:29]>C1COCC1>[CH3:27][S:28]([OH:31])(=[O:30])=[O:29].[CH3:10][CH:9]([CH3:22])[CH2:8][CH2:23][NH:25][CH2:10][C:16]1[CH:19]=[CH:20][C:13]2[O:12][C:11]3[CH:22]=[CH:9][C:8]([C:23]([NH2:25])=[O:24])=[CH:7][C:21]=3[CH2:18][CH2:17][C:14]=2[CH:15]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 131726648HCID 131726648, compound

Product 1

HCID 87756849HCID 87756849, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Dissolve amine of example 1 in THF (0.1M solution). Add metanesulfonic acid (1 equiv). Isolate the white precipitate by vacuum filtration to obtain the title compound. 1H-NMR (CD3OD, 300 MHz): 7.90-7.87 (m, 2H), 7.51-7.37 (m, 4H), 4.31 (s, 2H), 3.36 (s, 4H), 3.22-3.19 (m, 2H), 2.87 (s, 3H), 1.86-1.73 (m, 3H), 1.14 (d, 6H, J=6.5 Hz). Electrospray MS M+1 ion=339.

Workup

  1. customIsolate the white precipitate
  2. filtrationby vacuum filtration

Sources & evidence

ORD record
ord-58e09e7034084b7f84d47aef83182c42
Source dataset
uspto-grants-2007_10
Patent number
US07288543B2

Reaction notes

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