Diethyl Ether → 74137-66-9

HRID 325288Notes

Reaction equation

HRID 325288 reaction equation
[CH3:1][CH:2]([CH2:4][C@H:5]1[N:14]2[C:15]([C@@:17]([NH:22][C:23]([C@@H:25]3[CH:40]=[C:39]4[C@H:28]([CH2:29][C:30]5[C:38]6[C:33](=[CH:34][CH:35]=[CH:36][C:37]=64)[NH:32][CH:31]=5)[N:27]([CH3:41])[CH2:26]3)=[O:24])([CH:19]([CH3:21])[CH3:20])[O:18][C@@:13]2([OH:42])[C@H:12]2[N:8]([CH2:9][CH2:10][CH2:11]2)[C:6]1=[O:7])=[O:16])[CH3:3].[CH3:43][S:44]([OH:47])(=[O:46])=[O:45].C(OCC)C>C(O)C>[CH3:3][CH:2]([CH2:4][C@H:5]1[N:14]2[C:15]([C@@:17]([NH:22][C:23]([C@@H:25]3[CH:40]=[C:39]4[C@H:28]([CH2:29][C:30]5[C:38]6[C:33](=[CH:34][CH:35]=[CH:36][C:37]=64)[NH:32][CH:31]=5)[N:27]([CH3:41])[CH2:26]3)=[O:24])([CH:19]([CH3:20])[CH3:21])[O:18][C@@:13]2([OH:42])[C@H:12]2[N:8]([CH2:9][CH2:10][CH2:11]2)[C:6]1=[O:7])=[O:16])[CH3:1].[CH3:43][S:44]([OH:47])(=[O:46])=[O:45]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 164640HCID 164640, compound

Product 1

HCID 305769074137-66-9

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ergocryptinine (2.30 g; 4 mmoles) was dissolved in absolute ethanol (20 ml), containing methanesulfonic acid (0.3 ml; 4.62 mmoles). The clear solution was poured into absolute diethylether (300 ml) while stirring. The precipitated salt was filtered off and dried in vacuo. Ergocryptinine methanesulfonate (2.5 g; 97.6% of the theory) with a melting point of 174°-175° C. was obtained.

Workup

  1. filtrationThe precipitated salt was filtered off
  2. customdried in vacuo
  3. custom97.6% of the theory) with a melting point of 174°-175° C. was obtained

Sources & evidence

ORD record
ord-13ed57550fcf445a80823e8bcb25fded
Source dataset
uspto-grants-1984_04
Patent number
US04440772

Reaction notes

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