Diethyl Ether → 74137-64-7

HRID 325286Notes

Reaction equation

HRID 325286 reaction equation
[CH3:1][CH:2]([C@@:4]1([NH:26][C:27]([C@H:29]2[CH:44]=[C:43]3[C@@H:32]([CH2:33][C:34]4[C:42]5[C:37](=[CH:38][CH:39]=[CH:40][C:41]=53)[NH:36][CH:35]=4)[N:31]([CH3:45])[CH2:30]2)=[O:28])[O:17][C@:16]2([OH:18])[N:7]([C@@H:8]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:9]([N:11]3[C@H:15]2[CH2:14][CH2:13][CH2:12]3)=[O:10])[C:5]1=[O:6])[CH3:3].[CH3:46][S:47]([OH:50])(=[O:49])=[O:48].C(OCC)C>C(O)C>[CH3:3][CH:2]([C@@:4]1([NH:26][C:27]([C@@H:29]2[CH:44]=[C:43]3[C@H:32]([CH2:33][C:34]4[C:42]5[C:37](=[CH:38][CH:39]=[CH:40][C:41]=53)[NH:36][CH:35]=4)[N:31]([CH3:45])[CH2:30]2)=[O:28])[O:17][C@:16]2([OH:18])[N:7]([C@H:8]([CH2:19][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[C:9]([N:11]3[C@H:15]2[CH2:14][CH2:13][CH2:12]3)=[O:10])[C:5]1=[O:6])[CH3:1].[CH3:46][S:47]([OH:50])(=[O:49])=[O:48]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 7067483Ergocristinine

Product 1

HCID 305768874137-64-7

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ergocristinine (1.25 g; 0.05 mmoles) was dissolved in absolute ethanol (25 ml), containing methanesulfonic acid (0.15 ml; 2.31 mmoles). After clarifying, the solution was slowly poured into absolute diethylether (350 ml) while stirring. The precipitated salt was filtered off and dried in vacuo. Ergocristinine methanesulfonate (1.40 g; 96.4% of the theory) with a melting point of 170°-180° C. was obtained.

Workup

  1. filtrationThe precipitated salt was filtered off
  2. customdried in vacuo
  3. custom96.4% of the theory) with a melting point of 170°-180° C. was obtained

Sources & evidence

ORD record
ord-f7cb106a93e245edb271680fa5c991bc
Source dataset
uspto-grants-1984_04
Patent number
US04440772

Reaction notes

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