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Triethylamine → HCID 54547883, compound

HRID 361489
Notes
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Reaction equation

HRID 361489 reaction equation
[CH2:1]([OH:7])[CH2:2][CH2:3][CH:4]=[CH:5][CH3:6].[CH3:8][S:9](Cl)(=[O:11])=[O:10].C(N(CC)CC)C>ClCCl>[CH3:8][S:9]([O:7][CH2:1][CH2:2][CH2:3][CH:4]=[CH:5][CH3:6])(=[O:11])=[O:10]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 61370Hex-4-en-1-ol

Product 1

HCID 54547883HCID 54547883, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

This example illustrates a synthesis of 1-(4,5-Oxohexyl)-3,7-dimethylxanthine (inventive compound no. 1555). To a solution of 4-hexen-1-ol (1.22 g, 12.2 mmol) and methanesulfonyl chloride (1.04 mL, 13.4 mmol) in dichloromethane (15 mL), cooled in an ice bath, was added triethylamine (2.55 mL, 18.3 mmol) dropwise. After 5 minutes, the cooling bath was removed and the mixture stirred for an additional 45 minutes and then treated with saturated aqueous sodium bicarbonate solution (25 mL). The layers were separated and the aqueous layer extracted with dichloromethane (20 mL). The combined organic layers were dried over magnesium sulfate and the solvents evaporated under vacuum, yielding 1-methanesulfonyloxy-4-hexene as a viscous oil.

Workup

  1. customthe cooling bath was removed
  2. additiontreated with saturated aqueous sodium bicarbonate solution (25 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer extracted with dichloromethane (20 mL)
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. customthe solvents evaporated under vacuum

Sources & evidence

ORD record
ord-4c4b634d10a24d28b88d9c8b46642a63
Source dataset
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05866576

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes