Diethyl Ether → 74137-67-0

HRID 325289Notes

Reaction equation

HRID 325289 reaction equation
[CH3:1][CH:2]([CH2:4][C@@H:5]1[N:14]2[C:15]([C@@:17]([NH:20][C:21]([C@@H:23]3[CH:38]=[C:37]4[C@@H:26]([CH2:27][C:28]5[C:36]6[C:31](=[CH:32][CH:33]=[CH:34][C:35]=64)[NH:30][CH:29]=5)[N:25]([CH3:39])[CH2:24]3)=[O:22])([CH3:19])[O:18][C@@:13]2([OH:40])[C@H:12]2[N:8]([CH2:9][CH2:10][CH2:11]2)[C:6]1=[O:7])=[O:16])[CH3:3].[CH3:41][S:42]([OH:45])(=[O:44])=[O:43].C(OCC)C>C(O)C>[CH3:3][CH:2]([CH2:4][C@@H:5]1[N:14]2[C:15]([C@@:17]([NH:20][C:21]([C@@H:23]3[CH:38]=[C:37]4[C@H:26]([CH2:27][C:28]5[C:36]6[C:31](=[CH:32][CH:33]=[CH:34][C:35]=64)[NH:30][CH:29]=5)[N:25]([CH3:39])[CH2:24]3)=[O:22])([CH3:19])[O:18][C@@:13]2([OH:40])[C@H:12]2[N:8]([CH2:9][CH2:10][CH2:11]2)[C:6]1=[O:7])=[O:16])[CH3:1].[CH3:41][S:42]([OH:45])(=[O:44])=[O:43]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 105137Ergosine

Product 1

HCID 13556874137-67-0

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ergosinine (5.48 g; 10 mmoles) was dissolved in absolute ethanol (60 ml), containing methanesulfonic acid (0.72 ml; 11 mmoles). The clear solution was poured into absolute diethylether (600 ml). The precipitated salt was filtered off and dried in vacuo. Ergosinine methanesulfonate (6.05 g; 98.7% of the theory) with a melting point of 190°-192° C. was obtained.

Workup

  1. filtrationThe precipitated salt was filtered off
  2. customdried in vacuo
  3. custom98.7% of the theory) with a melting point of 190°-192° C. was obtained

Sources & evidence

ORD record
ord-d27947885c5c42f5b261b38e75f16ad1
Source dataset
uspto-grants-1984_04
Patent number
US04440772

Reaction notes

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