Triethylamine → HCID 131714665, compound

HRID 980799Notes

Reaction equation

HRID 980799 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[CH:13]([CH2:14][OH:15])[CH2:12][C:11]2=[CH:16][CH:17]=1.C(N(CC)CC)C>C(Cl)Cl>[S:2]([OH:4])(=[O:7])(=[O:3])[CH3:1].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[CH:13]([CH2:14][OH:15])[CH2:12][C:11]2=[CH:16][CH:17]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 13247995(4-Methoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl)methanol

Product 1

HCID 131714665HCID 131714665, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
0 °C

Procedure

Methane sulphonyl chloride (13.4 ml) is added dropwise to a stirred solution of 5-methoxy-1-hydroxymethyl benzocyclobutene (26 g) and triethylamine (26.5 ml) in methylene chloride (670 ml) cooled to 0° C. under nitrogen. The reaction mixture is allowed to warm to RT, stirred for 2 hours at RT, washed with water and saturated salt, dried over Na2SO4, and filtered. The filtrate is concentrated in vacuo yielding the desired product as a liquid.

Workup

  1. temperatureto warm to RT
  2. washwashed with water and saturated salt
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated in vacuo

Sources & evidence

ORD record
ord-44b4876a464e4f8780c58120eccea4af
Source dataset
uspto-grants-1987_01
Patent number
US04639442

Reaction notes

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