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Methyl iodide → HCID 87687587, compound

HRID 1396267
Notes
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Reaction equation

HRID 1396267 reaction equation
[CH2:1]([O:8][C@@H:9]1[C@@H:17]([C@@H:18]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:19]2SCCCS2)[O:16][C@H:15]2[C@H:11]([N:12]=[C:13]([N:33]([CH3:35])[CH3:34])[S:14]2)[C@H:10]1[O:36][CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=[O:45].[Ca+2].CI>CC(C)=O.O.ClCCl>[CH2:26]([O:25][C@H:18]([C@H:17]1[O:16][C@H:15]2[C@H:11]([N:12]=[C:13]([N:33]([CH3:35])[CH3:34])[S:14]2)[C@@H:10]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C@@H:9]1[O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH:19]=[O:45])[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 3

HCID 6328Methyl iodideHCID 10112Calcium CarbonateHCID 86701113HCID 86701113, compound

Product 1

HCID 87687587HCID 87687587, compound

Reagents, catalysts & solvents 3

HCID 180AcetoneSolventHCID 962Water
Solvent
HCID 6344DichloromethaneSolvent

Procedure

To a solution of 97 (3 g, 4.7 mmol) in acetone (16 mL) and water (4 mL) was added CaCO3 (4.7 g, 47 mmol) and CH3I (13.2 g, 94 mmol). After kept 20 hours at 50° C., the resulting solution was diluted with dichloromethane (30 mL), filtered and extracted with dichloromethane (2×30 mL). The combined organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford crude 98, which was used in next step directly; (ES, m/z) [M+H]+ 547.0.

Workup

  1. filtrationfiltered
  2. extractionextracted with dichloromethane (2×30 mL)
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto afford crude 98, which

Sources & evidence

ORD record
ord-b187874fde164f169813de93bff8e180
Source dataset
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08901087B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes