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Triethylamine → (Z)-Dec-4-en-1-yl methanesulfonate

HRID 530153
Notes
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Reaction equation

HRID 530153 reaction equation
[CH2:1]([OH:11])[CH2:2][CH2:3]/[CH:4]=[CH:5]\[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>ClCCl>[CH3:19][S:20]([O:11][CH2:1][CH2:2][CH2:3]/[CH:4]=[CH:5]\[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])(=[O:22])=[O:21]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 53627984-Decenol, (4Z)-

Product 1

HCID 89768212(Z)-Dec-4-en-1-yl methanesulfonateYield 95%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

To a cooled solution (0° C.) of (Z)-dec-4-en-1-ol 9 (20 g, 128.0 mmol) and triethylamine (26.7 mL, 191.9 mmol) in anhydrous dichloromethane (200 mL) was slowly added methane sulfonyl chloride (14.9 mL, 191.9 mmol). The solution was stirred for 30 min at room temperature then diluted with dichloromethane (100 mL). The solution was washed with saturated sodium bicarbonate (3×150 mL) and then the combined aqueous washes were extracted with dichloromethane (150 mL). The combined dichloromethane extracts were dried on magnesium sulfate, filtered and concentrated in vacuo to dryness. The residue was filtered through a pad of silica (100% dichloromethane) to afford (Z)-dec-4-enyl methanesulfonate 2 as a yellow oil (28.5 g, 95%). Rf 0.5 (100% CH2Cl2).

Workup

  1. washThe solution was washed with saturated sodium bicarbonate (3×150 mL)
  2. extractionthe combined aqueous washes were extracted with dichloromethane (150 mL)
  3. dry with materialThe combined dichloromethane extracts were dried on magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo to dryness
  6. filtrationThe residue was filtered through a pad of silica (100% dichloromethane)

Sources & evidence

ORD record
ord-8b317f2f5eb341bab3c77b307320e156
Source dataset
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09352042B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes